WO2023231292A1 - Beet pulp all-component emulsifying thickener, preparation method therefor, and application thereof - Google Patents

Beet pulp all-component emulsifying thickener, preparation method therefor, and application thereof Download PDF

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Publication number
WO2023231292A1
WO2023231292A1 PCT/CN2022/128828 CN2022128828W WO2023231292A1 WO 2023231292 A1 WO2023231292 A1 WO 2023231292A1 CN 2022128828 W CN2022128828 W CN 2022128828W WO 2023231292 A1 WO2023231292 A1 WO 2023231292A1
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beet pulp
water
beet
sugar beet
component
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PCT/CN2022/128828
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French (fr)
Chinese (zh)
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曾新安
林嘉伟
蔡锦林
韩忠
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华南理工大学
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Publication of WO2023231292A1 publication Critical patent/WO2023231292A1/en

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C13/00—Cream; Cream preparations; Making thereof
    • A23C13/12—Cream preparations
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/12—Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13—Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/1307—Milk products or derivatives; Fruit or vegetable juices; Sugars, sugar alcohols, sweeteners; Oligosaccharides; Organic acids or salts thereof or acidifying agents; Flavours, dyes or pigments; Inert or aerosol gases; Carbonation methods
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/12—Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13—Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/137—Thickening substances
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/244—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
    • Y02P60/87—Re-use of by-products of food processing for fodder production

Definitions

  • the present invention relates to an emulsifying thickener, in particular to a whole-component emulsifying thickener of sugar beet pulp and its preparation method and application; the soluble sugar beet obtained by converting the whole component of sugar beet pulp into an emulsifying thickening agent
  • the pectin component and insoluble nanofiber filaments have good emulsification and thickening properties, realizing the full utilization of all components of sugar beet meal.
  • Sugar beets are mainly produced in Xinjiang and Inner Mongolia in China. In 2020, my country's sugar beet production will be approximately 12 million tons. Beet meal is the main by-product of the beet sugar industry. Its dry meal output is 10% of the fresh weight. It is mainly produced through extrusion and granulation after beet juice extraction, and its acquisition cost is low. The dry basis of sugar beet pulp contains 25% ⁇ 30% pectin, 20% ⁇ 25% hemicellulose, 23% ⁇ 28% cellulose and 10% ⁇ 13% protein. It is currently mainly used in animal feed. Its rich polysaccharide resources have not been utilized industrially.
  • beet pulp Even if it is used in animal feed, beet pulp contains a variety of anti-nutritional factors such as free acids, thioglucosides, betaine and nitrates, which can cause damage to the health of animals, so its use in feed also has certain limitations. restrictions, we need to find more reasonable and efficient ways to utilize them.
  • the pectin in beet pulp has excellent emulsifying activity that other sources of pectin do not have. Compared with gum arabic, which is the "gold standard" of emulsifiers, its dosage is 1/10 of gum arabic to achieve results similar to gum arabic. emulsifying activity.
  • sugar beet pectin has problems with insufficient emulsion stability, and its adsorption efficiency at the oil-water interface is low.
  • long-term industrialized hot acid extraction will destroy the acid-sensitive neutral sugar side chains and make them connect with neutral sugars.
  • the hydrophobic protein breaks off and degrades from the sugar beet pectin molecules, thereby damaging its emulsifying activity and emulsifying stability.
  • sugar beet pulp will still produce secondary waste meal rich in dietary fiber, accounting for 55% of its initial mass. How to rationally utilize sugar beet meal and its secondary waste meal is still urgently needed. solved problem.
  • Chinese invention patent application CN201410326603.0 discloses a method for extracting sugar beet pectin by salt method
  • CN201410142256.6 discloses a microwave-assisted salt method for extracting sugar beet pectin
  • Chinese invention patent application CN201610575893 .1 discloses a method for large-scale production of sugar beet pectin, but these existing technologies do not pay attention to the subsequent treatment of secondary waste meal.
  • Chinese invention patent CN201610392264.5 discloses a method that uses steam explosion pretreatment to remove pectin and hemicellulose in the cell wall, and then uses hydrogen peroxide and high-intensity ultrasonic treatment to simultaneously obtain sugar beet pectin and nanocellulose.
  • this technology simply uses steam explosion method to separate pectin, and the yield is not high, and the insoluble fiber needs to be treated with hydrogen peroxide subsequently, and the components except cellulose are destroyed and not recycled.
  • the above-mentioned prior art chemical modification and compounding operations after extraction and purification further increase the preparation cost of cellulose Pickering emulsifier and limit its market application.
  • Chinese invention patent application CN201811377985.4 discloses a method for preparing nanoscale insoluble soybean polysaccharide by hydrothermal-ultrasonic crushing method, using pH The weak acid of 3.5 was used to remove soluble polysaccharides from soybean meal, and only nanoparticles of insoluble soybean polysaccharides were obtained.
  • Chinese invention patent application CN202110463660.3 discloses a method that uses a traditional hot acid method to separate pectin, and then uses a colloid mill and enzymatic method to crush citrus dietary fiber to prepare nanoparticle-sized citrus fiber with Pickering emulsification properties.
  • the existing technology has the following problems: 1)
  • the long-term hot acid extraction method used in industrial production can easily destroy the acid-sensitive neutral sugar side chains, causing the hydrophobic protein components connected to them to be degraded and damaging the beet pectin.
  • the amphiphilicity reduces its emulsifying activity; 2)
  • the physical stripping effect of ultrasonic cavitation is ignored to promote the dissolution of sugar beet meal;
  • the insufficient utilization of secondary waste meal after sugar beet pectin extraction leads to the waste of resources; 4
  • Cellulose used in Pickering emulsification requires a tedious separation and purification process and must be repeatedly modified or compounded with other substances to have good Pickering emulsification.
  • the present invention aims to expand the application field of beet pulp, provide a food-grade method to convert all components of beet pulp into an emulsifying thickening agent, and a preparation method thereof to achieve Full utilization of sugar beet meal resources.
  • Another object of the present invention is to provide the application of the whole-component emulsifying thickener of beet pulp for emulsifying and thickening fat-containing sauces, cream or yogurt.
  • a method for preparing a full-component emulsifying thickener of beet pulp including the following steps:
  • step 3 Add water to dilute the hydrothermally treated beet pulp dispersion obtained in step 2) and perform high-energy ultrasonic crushing while stirring;
  • step 4) Concentrate and then dry the ultrasonic crushed beet pulp dispersion obtained in step 3) to obtain a full-component emulsifying thickener of sugar beet pulp.
  • the cleaning and grinding pretreatment is to soak the pressed beet pulp in water until the beet shreds absorb water, swell and disperse, remove impurities including soil and sawdust and burnt beet shreds, and then sweeten the sugar beet shreds.
  • the rapeseed meal is taken out of the water, part of the water is removed, and then dried. The dried beet pulp is crushed and sieved and placed in a cool place for later use.
  • the removal of part of the water is carried out using a screw extruder; the drying is carried out in an oven; the drying temperature is controlled to be 45 ⁇ 65°C and the time is 10 ⁇ 24 h.
  • the moisture content is 6wt% ⁇ 9wt%.
  • the mesh size of the crushed and sieved dried sugar beet pulp is 100 to 400 mesh.
  • the concentration of the sugar beet pulp suspension formed by dispersing the washed, crushed and pretreated sugar beet pulp powder in water is 2wt% ⁇ 20wt%.
  • the hydrothermal treatment temperature is 120 ⁇ 130°C and the time is 1-1.5 h.
  • the concentration of the hydrothermally treated beet pulp dispersion diluted with water is 0.5wt% ⁇ 5wt%; the power density of the high-energy ultrasonic crushing treatment is 127 ⁇ 255 W/cm 2 and the time is 5 ⁇ 25 min;
  • the high-energy ultrasonic crushing treatment mode used is 2 s continuous and 2 s intervals.
  • the hydrothermal treatment beet pulp dispersion is mechanically stirred at a speed of 200 to 600 rpm. The stirring is carried out in an open container to mix a small amount of air bubbles into the system. , and use a -4 ⁇ 4°C circulating ice water bath to cool the system so that the system temperature is not higher than 45°C.
  • the concentration method adopts reduced pressure concentration or ultrafiltration membrane filtration and concentration; when concentrated to 13wt% ⁇ 15wt%, spray drying is used for drying.
  • a kind of beet pulp full-component emulsification thickener prepared by the above preparation method.
  • the soluble component content of the obtained sugar beet pulp whole-component emulsification thickener is 39.5wt% ⁇ 45.1wt%, and the soluble pectin content It is 24.3wt% ⁇ 29.7wt%.
  • the molecular weight of soluble pectin is 392 ⁇ 561kDa and contains fragrance.
  • the fiber is a strip-shaped nanofiber filament with a diameter of 50 ⁇ 200 nm and a length of 3 ⁇ 50 ⁇ m.
  • the present invention has the following advantages:
  • the present invention mainly performs hydrothermal treatment on sugar beet pulp, and then performs stirring and high-energy ultrasonic crushing treatment to dissociate the dense sugar beet pulp fibers into insoluble nanofibers and soluble macromolecular sugar beet pectin components.
  • This method reduces the degradation of sugar beet pectin during the dissolution process and protects its soluble colloidal emulsification properties; at the same time, it promotes the dissociation of nanofibers and enhances its Pickering emulsification properties as an insoluble solid.
  • the present invention uses hydrothermal softening of dense cell walls and stirring to enhance ultrasonic cavitation to peel off pectin to obtain sugar beet pectin with a low degree of degradation and protect its macromolecular structure and amphiphilicity.
  • the present invention uses soluble pectin and insoluble nanofibers together as a full-component emulsification thickener without separation, realizing 100% utilization of sugar beet pulp.
  • the nanofiber silk obtained by the present invention does not require deep separation, purification or further modification and compounding, and has Pickering emulsification effect.
  • the process does not require acid and alkali strong oxidants and enzymes, and is green and environmentally friendly.
  • the nanofiber silk of the present invention can exert a synergistic emulsification effect with sugar beet pectin.
  • the nanofiber silk has bending flexibility and can fit on the surface of oil droplets to form a staggered fiber network adsorption layer, and its gaps are filled with surface-active pectin. Covered, the two co-adsorb at the oil-water interface, forming a tight interfacial film at the oil-water interface.
  • the spatial barrier effect of the insoluble nanofibers significantly prevents oil droplets from contacting each other, overcoming the problem of poor emulsification stability of sugar beet pectin.
  • the present invention uses hydrothermal-ultrasonic treatment to peel off pectin, which is rich in content and has good emulsifying activity in the cell wall of beet pulp, and at the same time separates the beet fiber component into nanofiber filaments with Pickering emulsification properties to avoid acid
  • the use of strong alkali oxidants is environmentally friendly.
  • the present invention uses high-energy ultrasonic crushing technology to protect the macromolecular structure of beet pectin in the soluble polysaccharide/insoluble fiber mixed system; without the need for deep extraction and purification of cellulose, the soluble pectin and cellulose nanofilaments with synergistic emulsification effect are combined at the same time.
  • As a complete component of sugar beet meal it is used as an emulsification thickener to overcome the problem of poor emulsification stability of sugar beet pectin and achieve full utilization of sugar beet meal.
  • the present invention adopts a one-pot method, which has a simple process and few separation and purification operations. No additional chemical reagents are needed. It is green and non-toxic.
  • the product usage method is simple and can be applied to the food industry.
  • Figure 1 is a schematic diagram of the high-energy ultrasonic treatment equipment used in the present invention.
  • Figure 2 is an atomic microscope image of the insoluble fiber of the product obtained in Example 1.
  • Figure 3 is an optical microscope picture of the original sugar beet pulp in Example 1.
  • Figure 4 shows the appearance of the product suspension and the original sugar beet pulp powder suspension in Example 1.
  • Figure 5 is an optical microscope picture of the emulsion prepared from the product of Example 1.
  • Figure 6 is an optical microscope image of the emulsion prepared in Comparative Example 1.
  • Figure 7 is a diagram of the emulsification mechanism of the emulsion (a) prepared by the product of Example 1 and the emulsion (b) prepared by Comparative Example 1.
  • Figure 8 is an optical microscope image of insoluble particles of the product obtained in Comparative Example 1.
  • Figure 9 shows the appearance of the product suspension of Comparative Example 1 (a) and the appearance of the original sugar beet pulp powder suspension (b).
  • beet pulp is first subjected to hydrothermal treatment, and then subjected to stirring and high-energy ultrasonic crushing treatment.
  • the beet pulp is rich in pectin components with good emulsification properties.
  • hydrothermal treatment the chemical bonds of the compounds covalently bound to the cell wall are broken.
  • the pectin and hemicellulose components dissolve, causing the originally dense cell wall tissue structure to become porous and loose, causing swelling and an increase in the specific surface area.
  • a rough surface with a large specific surface area can reduce the cavitation threshold of ultrasound, provide more cavitation bubble nucleation sites for the high-energy ultrasound (127-255 W/cm 2 ) process, and can achieve the desired effect on the surface and interior of rough porous sugar beet pulp.
  • a large number of cavitation bubbles are generated and impact the beet pulp to dissociate it into fiber filaments with a diameter of nanometer level and a length of tens of microns.
  • the system of the present invention is mixed with dissolved pectin and insoluble sugar beet pulp particles (total concentration is 0.5wt%-5wt%).
  • the porous sugar beet pulp not only promotes the ultrasonic cavitation process, but also absorbs most of the ultrasonic energy and has been dissolved.
  • the macromolecular sugar beet pectin was protected from significant degradation because it did not absorb enough ultrasound energy.
  • the mechanical stirring (200-600 rpm) of the ultrasonic process mixes a small amount of air into the system, so that ultrasonic cavitation bubbles can be continuously replenished and generated.
  • Hydrothermal pretreatment and stirring high-energy ultrasonic treatment play a synergistic role in the crushing process of sugar beet pulp.
  • Disperse the product in water to prepare a suspension with a concentration of 3wt% use a high-speed shear instrument to disperse at 20,000 rpm for 5 minutes, and then mechanically stir for 5 hours to fully disperse.
  • the suspension was centrifuged at 10,000 g for 30 min, take the supernatant. After the supernatant is freeze-dried, the dried soluble content is weighed. The ratio of the total soluble content to the dry weight of the original product is the soluble content ratio. Take the freeze-dried solubles and perform a Kjeldahl nitrogen test to determine the protein content in the solubles.
  • the protein conversion coefficient is 6.25.
  • the ratio of the total protein to the dry weight of the original product is the soluble protein content.
  • High performance liquid chromatography-size exclusion chromatography was used to determine the molecular weight of sugar beet pectin.
  • the chromatographic column was Ultrahydrogel. Guard, Ultrahydrogel 2000 and Ultrahydrogel 1000 are used together with three columns, using a refractive index detector, and the mobile phase is 0.1 mol/L sodium nitrate solution (containing 0.05wt% sodium azide), flow rate is 0.6 mL/min, temperature 35°C, injection volume 100 ⁇ L.
  • Dextran standards with molecular weights of 4400 to 667000 Da were used as standard curves for relative molecular weight quantification.
  • the apparent viscosity of the product suspension was measured using a TA rotational rheometer equipped with a 40mm diameter flat plate rotor. The measurement conditions are 10/s and the temperature is 25°C.
  • the emulsion particle size d 4,3 was measured using a Malvern MS3000 laser particle size analyzer. Using water as the dispersion medium, measure the particle size of freshly prepared emulsion and the particle size of emulsion that has been sealed and stored at room temperature for 60 days. The greater the change in emulsion particle size d 4,3 , the worse the emulsion stability.
  • Preparation Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 65°C for 10 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation.
  • the obtained sugar beet pulp suspension is cooled to normal temperature and then water is added to dilute the sugar beet pulp to a concentration of about 5wt%.
  • the total volume is 5 L.
  • the probe-type high-energy ultrasonic method is used to crush the sugar beet pulp.
  • the ultrasonic power is 127 W/ cm 2 , treatment time 30 min, ultrasonic duration 2 s, interval 2 s.
  • mechanical stirring at 600 rpm was used to mix a small amount of bubbles into the system so that the system was evenly treated by ultrasonic and cooled with an ice-water bath to make the suspension in The temperature during processing should not exceed 45°C.
  • the obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt% ⁇ 15wt% and then spray-dried to obtain the beet pulp full-component emulsifying thickener of Example 1.
  • the product powder of Example 1 is dispersed in water to form a suspension with a concentration of 5wt%.
  • the suspension is homogenized using high-speed shear homogenization method.
  • the rotation speed is 19000 ⁇ 20000 rpm.
  • the homogenization time is 8 minutes.
  • use Mechanical stirring was performed at 450 ⁇ 500 rpm for 15 h.
  • the obtained suspension can be diluted or directly used for emulsification and thickening; for example, the full-component emulsification thickener in this embodiment is suitable for the preparation of salad dressing/mayonnaise.
  • the full-component emulsifying thickener of this embodiment can significantly increase the content of dietary fiber in the sauce, and increase the viscosity of the sauce and the stability of the emulsion by forming a spatial network structure. , delaying the digestion of oil and reducing the digestibility of oil to achieve the goal of reducing oil.
  • the obtained full-component emulsifying thickener can also be used in cream whipping. Compared with common mono/diglycerol fatty acid esters, this product can prepare cream products with better plasticity.
  • the full-component emulsifying thickener The fiber network structure formed by the thickener makes the emulsion more stable.
  • the soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in Example 1 is 39.5wt%, of which the soluble pectin component content is 24.3wt%, and the molecular weight of the soluble pectin is 561 kDa, as shown in Table 1 .
  • the insoluble components dissociate into nanofiber filaments with diameters of 50 to 200 nm and lengths of 3 to 50 ⁇ m (as shown in the atomic force microscope photo in Figure 2).
  • the obtained product appears as uniform and non-stratified fibrous colloid floc (Figure 3), with good colloid stability, while the original sugar beet pulp has obvious stratification and almost no swelling (b, Figure 4)
  • Figure 4 is the appearance of the product suspension of Example 1), and its optical microscope photo shows that it is massive particles with a diameter of more than ten to tens of microns and regular edges on the surface ( Figure 3);
  • 0.5wt% The apparent viscosity of the product in this example is 1.153 Pa ⁇ s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa ⁇ s and 0.022 Pa ⁇ s.
  • the product in this example has good thickening sex.
  • the product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion.
  • the emulsion particle size d 4,3 is 6.24 ⁇ m.
  • the emulsion particle size d 4,3 is 6.31 ⁇ m. No obvious emulsion stratification occurred, and the emulsification stability was good.
  • the micrograph of the emulsion prepared by the product of this example shows that its surface is smooth (Figure 5).
  • the fiber filaments with a diameter of nanometers are transparent at the interface and cannot be directly observed.
  • the formation mechanism of the emulsion is shown in a in Figure 7.
  • the nanofiber filaments are interlaced to form a network structure that adheres to the emulsion interface, and the gaps are covered by soluble pectin, forming a tight network interface film structure, which synergistically maintains the stability of the emulsion.
  • a 20wt% corn oil emulsion of beet pectin was prepared separately at a concentration of 0.5wt%.
  • the emulsion particle size d 4,3 was 1.16 ⁇ m.
  • the emulsion particle size d 4,3 was 35.2 ⁇ m after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
  • Preparation Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 45°C for 24 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation.
  • the obtained sugar beet pulp suspension is cooled to normal temperature and then water is added to dilute the sugar beet pulp to a concentration of approximately 0.5wt%.
  • the total volume is 2L.
  • the probe-type high-energy ultrasonic method is used to crush the sugar beet pulp.
  • the ultrasonic power is 255 W/cm 2
  • the treatment time is 5 min
  • the ultrasonic duration is 2 s
  • the interval is 2 s.
  • mechanical stirring at 200 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath.
  • the temperature of the suspension should not exceed 45°C during treatment.
  • the obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt% ⁇ 15wt% and then spray-dried to obtain a full-component emulsified thickening agent for sugar beet pulp.
  • the product powder is dispersed in water to form a suspension with a concentration of 0.8wt%.
  • the suspension is homogenized using high-speed shear homogenization method with a rotation speed of 19000 ⁇ 20000. rpm, the homogenization time is 2 minutes, and then mechanical stirring is used at 450 ⁇ 500 Stir at rpm for 5 h.
  • the resulting suspension can be diluted or directly used for emulsification and thickening.
  • the soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in this example is 45.1wt%, of which the soluble pectin component content is 29.7wt%, and the molecular weight of the soluble pectin is 392 kDa, as shown in Table 1.
  • the insoluble components are dissociated into nanofibers with diameters of 50 to 200 nm and lengths of 3 to 50 ⁇ m.
  • the obtained product appears as a uniform non-stratified fibrous colloid floc with good colloid stability, while the original sugar beet pulp is obviously stratified and almost does not swell, showing a massive structure; 0.5wt%
  • the apparent viscosity of the product in this example is 1.361 Pa ⁇ s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa ⁇ s and 0.019 Pa ⁇ s.
  • the product in this example has good thickening sex.
  • the product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion.
  • the emulsion particle size d 4,3 is 5.73 ⁇ m.
  • the emulsion particle size d 4,3 is 5.80 ⁇ m. No obvious emulsion stratification occurred, and the emulsification stability was good.
  • a 20wt% corn oil emulsion of beet pectin was prepared separately at a concentration of 0.5wt%.
  • the emulsion particle size d 4,3 was 1.36 ⁇ m.
  • the emulsion particle size d 4,3 was 28.8 ⁇ m after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
  • Preparation Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 55°C for 15 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation.
  • the ultrasonic power is 190 W/cm 2
  • the treatment time is 12 min
  • the ultrasonic duration is 2 s
  • the interval is 2 s.
  • mechanical stirring at 400 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath.
  • the temperature of the suspension should not exceed 45°C during treatment.
  • the obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt% ⁇ 15wt% and then spray-dried to obtain a full-component emulsified thickening agent for sugar beet pulp.
  • the product powder is dispersed in water to form a suspension with a concentration of 2.5wt%.
  • the suspension is homogenized using high-speed shear homogenization method with a rotation speed of 19000 ⁇ 20000. rpm, the homogenization time is 5 minutes, and then mechanical stirring is used at 450 ⁇ 500 Stir at rpm speed for 8 h.
  • the resulting suspension can be diluted or directly used for emulsification and thickening.
  • the soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in this example is 43.2wt%, of which the soluble pectin component content is 28.6wt%, and the molecular weight of the soluble pectin is 459 kDa, as shown in Table 1.
  • the insoluble components dissociate into nanofiber filaments with diameters of 50 to 200 nm and lengths of 3 to 50 ⁇ m.
  • the obtained product appears as a uniform non-stratified fibrous colloid floc with good colloid stability, while the original sugar beet pulp is obviously stratified and almost does not swell, showing a massive structure; 0.5wt%
  • the apparent viscosity of the product in this example is 1.225 Pa ⁇ s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa ⁇ s and 0.021 Pa ⁇ s.
  • the product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion.
  • the emulsion particle size d 4,3 is 6.13 ⁇ m.
  • the emulsion particle size d 4,3 is 6.18 ⁇ m. No obvious emulsion stratification occurred, and the emulsification stability was good.
  • 20wt% corn oil liquid was prepared separately from sugar beet pectin at a concentration of 0.5wt%.
  • the emulsion particle size d 4,3 was 1.21 ⁇ m.
  • the emulsion particle size d 4,3 was 25.5 ⁇ m after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
  • Preparation impurity removal, drying, and crushing are the same as in Example 1.
  • the obtained sugar beet pulp powder (passed through a 100-mesh sieve) is dispersed with water to form a sugar beet pulp with a concentration of approximately 5 wt% and a total volume of 5 L.
  • the sugar beet pulp is then crushed using a probe-type high-energy ultrasonic method.
  • the ultrasonic power is 127 W/cm 2
  • the treatment time is 30 min
  • the ultrasonic duration is 2 s
  • the interval is 2 s.
  • mechanical stirring at 600 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath.
  • the temperature of the suspension should not exceed 45°C during treatment.
  • the obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt% ⁇ 15wt% and then spray-dried to obtain the emulsified thickener of Comparative Example 2.
  • the soluble solids ratio of the emulsified thickener prepared in this comparative example is 18.6wt%, of which the soluble pectin component is 10.2wt%, and the molecular weight of the soluble pectin is 516 kDa, as shown in Table 1. Its optical microscope photo shows that it is a massive particle with a diameter of more than ten to tens of microns and a regular edge on the surface (as shown in Figure 8).
  • the appearance of the obtained product is a sediment at a concentration of 0.5wt%, with poor colloidal stability, similar to the original sugar beet meal with obvious stratification
  • Figure 9, a in Figure 9 is the appearance of the product suspension of Comparative Example 1
  • Figure 9 b is the appearance of the original sugar beet meal powder suspension
  • the apparent viscosity of 0.5wt% of this comparative product is 0.011 Pa ⁇ s
  • the apparent viscosity of the original sugar beet meal and control sugar beet pectin at the same concentration is 0.008 Pa ⁇ s and 0.022 Pa ⁇ s
  • the product of this comparative example has poor thickening properties.
  • the product of this comparative example at a concentration of 0.5wt% can prepare a 20 wt% corn oil emulsion, but it rapidly stratifies after homogenization, and some oil is obviously separated out.
  • the emulsion particle size d 4,3 is 78.6 ⁇ m. , poor emulsifying activity.
  • Figure 6 is a microscope picture of the emulsion prepared in this comparative example. A large number of particles are not all adsorbed to the oil droplet interface, and only a small amount of spherical emulsion droplets are in the field of view.
  • the emulsion formation mechanism is shown in b in Figure 7.
  • the massive particles are not flexible, and their large diameter makes it difficult to adsorb to the surface of the oil droplets, and they cannot form a network structure with the water-soluble pectin co-adsorbed to the interface.
  • the interface film is fragile and the oil droplets are easily exposed, resulting in emulsion properties. Difference. After the emulsion was stored at room temperature for only 7 days, oil separation from the emulsion intensified and the particle size of the emulsion could not be determined, resulting in poor emulsion stability.
  • Preparation impurity removal, drying, and crushing are the same as in Example 1. Take the sugar beet pulp powder (passed through a 100 mesh sieve) and disperse it in water to form a sugar beet pulp suspension with a concentration of about 20wt%. Place it in a high-pressure reactor at 110 ⁇ 120 °C treatment for 4 h. The obtained suspension was diluted to a concentration of 13wt% to 15wt% and then spray-dried to obtain the emulsified thickener of Comparative Example 1.
  • the soluble solids ratio of the emulsified thickener prepared in this comparative example is 23.1wt%, of which the soluble pectin component content is 14.4wt%, and the molecular weight of the soluble pectin is 528 kDa, as shown in Table 1.
  • the insoluble components are massive particles with regular surfaces.
  • the obtained product appears as a sediment at a concentration of 0.5wt%, with poor colloidal stability, similar to the original sugar beet meal with obvious stratification; the apparent viscosity of the comparative product at 0.5wt% is 0.009 Pa ⁇ s, while the original sweetened The apparent viscosity of rapeseed meal and control sugar beet pectin at the same concentration are 0.008 Pa ⁇ s and 0.022 Pa ⁇ s.
  • the product of this comparative example has no thickening property.
  • the product of this comparative example at a concentration of 0.5wt% cannot produce stable 20
  • the wt% corn oil emulsion quickly stratifies and precipitates a large amount of oil after homogenization.
  • the particle size of the emulsion cannot be measured and it has no emulsifying ability.
  • Preparation impurity removal, drying, and crushing are the same as in Example 1. Disperse the sugar beet pulp powder in water to form a sugar beet pulp suspension with a concentration of approximately 20wt%, and place it in a high-pressure reaction kettle for treatment at 110 ⁇ 120°C for 4 hours. The obtained sugar beet pulp powder was dispersed with water to form a sugar beet pulp with a concentration of about 5wt% and a total volume of 5 L. The sugar beet pulp was then treated with low-energy ultrasonic treatment using a tank-type ultrasonic cleaner. The ultrasonic power was 0.88 W/cm 2 and the continuous ultrasonic treatment time was 30 min.
  • the soluble solids ratio of the emulsified thickener prepared in this comparative example is 26.7 wt%, of which the soluble pectin component content is 16.2 wt%, the molecular weight of soluble pectin is 532 kDa, as shown in Table 1.
  • the insoluble components are massive particles with regular surfaces.
  • the obtained product looks like a precipitate at a concentration of 0.5wt%, with poor colloidal stability, similar to the original beet meal with obvious stratification; the apparent viscosity of the 0.5wt% product is 0.013 Pa ⁇ s, while the original beet meal and the control The apparent viscosity of sugar beet pectin at the same concentration is 0.008 Pa ⁇ s and 0.022 Pa ⁇ s, and the product of this comparative example has poor thickening properties.
  • the product of this comparative example at a concentration of 0.5% cannot prepare a stable 20wt% corn oil emulsion. After homogenization, it rapidly stratifies and precipitates a large amount of oil. The particle size of the emulsion cannot be measured and it does not have emulsifying ability.
  • the combined treatment of electrostatic field (8 ⁇ 32kV) and weaker ultrasound (0.35 ⁇ 0.88W/cm 2 ) mentioned in the Chinese invention patent (CN20130381569.2) can promote the dissolution of pectin. It is used to extract beet pectin, but the weak ultrasonic effect cannot effectively break up the beet pulp and dissociate it into filamentous nanofibers. The remaining sugar beet pulp particles are still large particles with poor colloidal stability and poor emulsification.
  • the whole-component emulsifying thickener of beet pulp prepared by the invention not only contains soluble pectin molecules with large molecular weight and complete molecular structure, which have good emulsifying activity; it also contains nanometer-sized molecules with a length of tens of micrometers and a diameter of nanometers.
  • Fiber filaments have the characteristics of larger aspect ratio and good bending flexibility. They can freely bend and fit tightly on the surface of spherical oil droplets.
  • the granular sugar beet pulp that has not been dissociated into nanowires has a particle diameter of about several microns, and the area of its rigid particles adsorbed on the surface of the oil droplets is much smaller than that of nanowires with bending flexibility.
  • the adsorption energy exceed It is large and difficult to adsorb to the surface of oil droplets, and the amount of particles required to stabilize oil droplets of the same area is much larger than that of filamentous sugar beet pulp. Although it can be adsorbed on oil droplets together with soluble pectin, the particle size of its emulsion The larger the diameter, the more prone to delamination instability.
  • the nanometer-scale diameter reduces the adsorption energy of the filamentary fibers and quickly and closely adheres to the surface of the oil droplets, thereby forming an intertwined network interface film structure.
  • the gaps between the fiber filaments are covered by macromolecular pectin components, and the two work together to form a tight network interface film, which prevents the instability of oil droplets caused by exposure of oil droplets and improves the stability of the emulsion.
  • Chinese invention patent application CN202110463660.3 discloses a method that uses a traditional hot acid method to separate pectin, and then uses a colloid mill and enzymatic method to crush citrus dietary fiber to prepare nanoparticles with Pickering emulsification properties.
  • Citrus fiber Chinese invention patent application CN201811377985.4 discloses a method for preparing nanoscale insoluble soybean polysaccharide by hydrothermal-ultrasonic crushing method, using pH The weak acid of 3.5 was used to remove soluble polysaccharides from soybean meal, and only nanoparticles of insoluble soybean polysaccharides were obtained.
  • the present invention uses a hydrothermal physical method without the addition of chemical reagents to simultaneously obtain structurally intact macromolecular sugar beet pectin and completely dissociated nanofibers from sugar beet pulp.
  • the synergy of the two can achieve good emulsification and thickening.

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Abstract

Disclosed in the present invention are a beet pulp all-component emulsifying thickener, a preparation method therefor, and an application thereof. The preparation method comprises: firstly, performing cleaning and crushing pretreatment on beet pulp; dispersing beet pulp powder in water after the cleaning and crushing pretreatment, and placing a mixture in a high-pressure reaction kettle for hydrothermal treatment for 0.5-4 hours at a controlled temperature of 110-140°C; adding water for dilution, and then performing high-energy ultrasonic crushing treatment while stirring; and concentrating and drying to obtain the beet pulp all-component emulsifying thickener. According to the present invention, the whole process does not need acids, alkali, strong oxidants and enzymes, thereby achieving greenness and environmental friendliness; and nano-fiber filaments and beet pectin can play a synergistic emulsification effect and are jointly adsorbed to an oil-water interface to form a compact net-shaped interface film, thereby achieving a stronger steric hindrance barrier effect, solving the problem of poor emulsion stability of the beet pectin, and achieving all-component utilization of the beet pulp.

Description

一种甜菜粕全组分乳化增稠剂及其制备方法与应用A kind of beet pulp full-component emulsifying thickener and its preparation method and application 技术领域Technical field
本发明涉及一种乳化增稠剂，特别是涉及一种甜菜粕全组分乳化增稠剂及其制备方法与应用；将甜菜粕全组分转化为乳化增稠剂，获得的可溶性甜菜果胶组分及不溶性纳米纤维丝，具有良好的乳化性和增稠性，实现甜菜粕全组分的全利用。The present invention relates to an emulsifying thickener, in particular to a whole-component emulsifying thickener of sugar beet pulp and its preparation method and application; the soluble sugar beet obtained by converting the whole component of sugar beet pulp into an emulsifying thickening agent The pectin component and insoluble nanofiber filaments have good emulsification and thickening properties, realizing the full utilization of all components of sugar beet meal.
背景技术Background technique
甜菜在中国主产于新疆和内蒙古地区，2020年我国糖用甜菜产量约1200万吨。甜菜粕是甜菜糖产业的主要副产物，其干粕产量为鲜重的10%，主要在甜菜榨汁后通过挤压制粒生产，其获取成本低。甜菜粕干基中含有25%~30%的果胶，20%~25%的半纤维素，23%~28%的纤维素和10%~13%的蛋白质，目前主要用于动物饲料，其丰富的多糖资源并未得到产业化利用。即便是用于动物饲料，甜菜粕中含有的多种抗营养因子如游离酸、硫葡萄糖苷、甜菜碱和硝酸盐等会导致动物的健康受损，因此其在饲料中的使用也有一定的限制，需要寻求更多合理高效利用的方法。甜菜粕中的果胶具有其他来源果胶所不具备的优异乳化活性，与作为乳化剂“金标准”的***胶相比，其用量为***胶的1/10即可达到与***胶相似的乳化活性。但甜菜果胶在应用上存在乳化稳定性不足的问题，其在油水界面吸附效率较低，特别是工业化的长时间热酸提取会破坏酸敏感的中性糖侧链，使与中性糖连接的疏水性蛋白质从甜菜果胶分子上断裂降解而损害其乳化活性和乳化稳定性。与此同时，甜菜粕在经历甜菜果胶的提取以后仍会产生占其初始质量55%的富含膳食纤维的二次废粕，如何合理利用甜菜粕及其二次废粕仍是亟待解决的问题。Sugar beets are mainly produced in Xinjiang and Inner Mongolia in China. In 2020, my country's sugar beet production will be approximately 12 million tons. Beet meal is the main by-product of the beet sugar industry. Its dry meal output is 10% of the fresh weight. It is mainly produced through extrusion and granulation after beet juice extraction, and its acquisition cost is low. The dry basis of sugar beet pulp contains 25%~30% pectin, 20%~25% hemicellulose, 23%~28% cellulose and 10%~13% protein. It is currently mainly used in animal feed. Its rich polysaccharide resources have not been utilized industrially. Even if it is used in animal feed, beet pulp contains a variety of anti-nutritional factors such as free acids, thioglucosides, betaine and nitrates, which can cause damage to the health of animals, so its use in feed also has certain limitations. restrictions, we need to find more reasonable and efficient ways to utilize them. The pectin in beet pulp has excellent emulsifying activity that other sources of pectin do not have. Compared with gum arabic, which is the "gold standard" of emulsifiers, its dosage is 1/10 of gum arabic to achieve results similar to gum arabic. emulsifying activity. However, the application of sugar beet pectin has problems with insufficient emulsion stability, and its adsorption efficiency at the oil-water interface is low. In particular, long-term industrialized hot acid extraction will destroy the acid-sensitive neutral sugar side chains and make them connect with neutral sugars. The hydrophobic protein breaks off and degrades from the sugar beet pectin molecules, thereby damaging its emulsifying activity and emulsifying stability. At the same time, after the extraction of sugar beet pectin, sugar beet pulp will still produce secondary waste meal rich in dietary fiber, accounting for 55% of its initial mass. How to rationally utilize sugar beet meal and its secondary waste meal is still urgently needed. solved problem.
关于甜菜果胶分离及应用，中国发明专利申请CN201410326603.0公开了一种盐法提取甜菜果胶的方法、CN201410142256.6公开了一种微波辅助盐法提取甜菜果胶的方法和中国发明专利CN201610575893.1公开了一种大规模生产甜菜果胶的方法，但这些现有技术都没有关注后续二次废粕的处理。中国发明专利CN201610392264.5公开了一种采用蒸汽***预处理去除细胞壁内果胶和半纤维素，再采用双氧水和高强度超声处理的方法来同时获取得到甜菜果胶和纳米纤维素的方法。但该技术单纯采用蒸汽***方法来分离果胶的产率并不高，而且后续还需对不溶纤维进行了双氧水处理，除纤维素外的组分都被破坏而没有得到回收利用。Regarding the separation and application of sugar beet pectin, Chinese invention patent application CN201410326603.0 discloses a method for extracting sugar beet pectin by salt method, CN201410142256.6 discloses a microwave-assisted salt method for extracting sugar beet pectin, and Chinese invention patent application CN201610575893 .1 discloses a method for large-scale production of sugar beet pectin, but these existing technologies do not pay attention to the subsequent treatment of secondary waste meal. Chinese invention patent CN201610392264.5 discloses a method that uses steam explosion pretreatment to remove pectin and hemicellulose in the cell wall, and then uses hydrogen peroxide and high-intensity ultrasonic treatment to simultaneously obtain sugar beet pectin and nanocellulose. However, this technology simply uses steam explosion method to separate pectin, and the yield is not high, and the insoluble fiber needs to be treated with hydrogen peroxide subsequently, and the components except cellulose are destroyed and not recycled.
除单纯获取果胶和纤维素外，富含纤维的农副产物的一个重要的利用方向是将所得纤维素作为皮克林乳化剂。纤维素的提取需要繁杂的工序以及会消耗大量酸碱及强氧化性试剂。而且纯纤维素的亲水性过强而无法表现良好皮克林乳化性，需要进行化学改性或与其他疏水性物质进行复合，如中国发明专利申请CN201810460609.5公开的辐射法诱导苯乙烯接枝改性纤维素，中国发明专利申请CN201710088643.X公开的辛烯基琥珀酸接枝改性纤维素都属于上述情况。上述现有技术的提取纯化后进行化学改性及复合操作进一步推高纤维素皮克林乳化剂的制备成本，限制其市场化应用。In addition to simply obtaining pectin and cellulose, an important utilization direction of fiber-rich agricultural and sideline products is to use the obtained cellulose as Pickering emulsifier. The extraction of cellulose requires complicated processes and consumes a large amount of acids, bases and strong oxidizing reagents. Moreover, pure cellulose is too hydrophilic to exhibit good Pickering emulsification, and needs to be chemically modified or compounded with other hydrophobic substances. For example, the radiation method disclosed in Chinese invention patent application CN201810460609.5 induces styrene bonding. Branch-modified cellulose, and the octenylsuccinic acid graft-modified cellulose disclosed in Chinese invention patent application CN201710088643.X all fall into the above situation. The above-mentioned prior art chemical modification and compounding operations after extraction and purification further increase the preparation cost of cellulose Pickering emulsifier and limit its market application.
将提取程度低且组成复杂的膳食纤维直接用于皮克林稳定可以避免对纤维素进行提取-改性和直接实现植物农副产物全利用。中国发明专利申请CN201811637533.5公开了一种对豆渣进行酶解-水热-喷雾干燥的处理方法，将豆渣转化为水包油乳化剂。该方法除了需要用到生物制剂酶以外，豆渣只经过单纯的水热处理并不能有效破碎其细胞壁纤维结构，其所能发挥的皮克林稳定机制效果受限。中国发明专利申请CN201811377985.4公开了一种水热-超声破碎法制备纳米级不溶性大豆多糖的方法，采用pH 3.5的弱酸对大豆粕进行可溶性多糖的脱除，仅获得大豆不溶性多糖的纳米颗粒。中国发明专利申请CN202110463660.3公开了一种采用传统热酸法分离果胶，而后采用胶体磨及酶法来破碎柑橘膳食纤维，制备出具有皮克林乳化性的纳米粒径柑橘纤维。后两者均对不溶性纤维进行精制分离，只关注了不溶性纤维的乳化性而忽略了其与可溶性组可能存在的协同乳化增稠作用。现有技术也有利用了超声技术进行可溶或不可溶膳食纤维的提取，均利用了超声波对酸碱试剂及酶的强化作用，但均忽略了强化超声空化微射流的纯物理方式进行膳食纤维的促进溶解，如中国发明专利申请CN202110308407.0采用超声联用强碱和超声联用除盐剂进行拟球藻不溶性膳食纤维的提取，中国发明专利申请CN201710326415.1采用超声联用脂肪酶对石榴皮渣籽的不溶性膳食纤维进行提取。Directly using dietary fiber with a low degree of extraction and complex composition for Pickering stabilization can avoid the extraction and modification of cellulose and directly realize the full utilization of plant agricultural and sideline products. Chinese invention patent application CN201811637533.5 discloses a processing method of enzymatic hydrothermal-spray drying of bean dregs to convert the bean dregs into an oil-in-water emulsifier. In addition to the use of biological enzymes, this method cannot effectively break the cell wall fiber structure of bean dregs after simple hydrothermal treatment, and the Pickering stabilization mechanism it can exert is limited. Chinese invention patent application CN201811377985.4 discloses a method for preparing nanoscale insoluble soybean polysaccharide by hydrothermal-ultrasonic crushing method, using pH The weak acid of 3.5 was used to remove soluble polysaccharides from soybean meal, and only nanoparticles of insoluble soybean polysaccharides were obtained. Chinese invention patent application CN202110463660.3 discloses a method that uses a traditional hot acid method to separate pectin, and then uses a colloid mill and enzymatic method to crush citrus dietary fiber to prepare nanoparticle-sized citrus fiber with Pickering emulsification properties. The latter two both refined and separated insoluble fiber, focusing only on the emulsifying properties of insoluble fiber and ignoring its possible synergistic emulsification and thickening effect with the soluble group. Existing technologies also use ultrasonic technology to extract soluble or insoluble dietary fiber. They all use the strengthening effect of ultrasonic waves on acid-base reagents and enzymes, but they all ignore the purely physical method of enhancing ultrasonic cavitation microjet to extract dietary fiber. Promote dissolution. For example, Chinese invention patent application CN202110308407.0 uses ultrasound combined with strong alkali and ultrasound combined with desalting agent to extract insoluble dietary fiber of Nannochloropsis. Chinese invention patent application CN201710326415.1 uses ultrasound combined with lipase to extract pomegranate. Extract the insoluble dietary fiber from the seeds.
总体来说，现有技术存在以下问题：1）工业化生产采用长时间热酸提取法容易破坏酸敏感的中性糖侧链，使与之相连的疏水性蛋白质组分被降解，损害甜菜果胶的两亲性而降低其乳化活性；2）忽略了超声波空化作用的物理剥离对甜菜粕的促进溶解作用；3）甜菜果胶提取后二次废粕利用不足导致资源浪费的问题；4）纤维素用于皮克林乳化需要繁琐分离纯化过程且还要重复改性或与其他物质复合才能具有良好皮克林乳化性，该过程需要使用大量酸，碱，强氧化剂和酶制剂，成本高且环境不友好；5）甜菜果胶乳化稳定性差；6）忽略纤维皮克林乳化剂与可溶性组分之间的协同乳化作用。Generally speaking, the existing technology has the following problems: 1) The long-term hot acid extraction method used in industrial production can easily destroy the acid-sensitive neutral sugar side chains, causing the hydrophobic protein components connected to them to be degraded and damaging the beet pectin. The amphiphilicity reduces its emulsifying activity; 2) The physical stripping effect of ultrasonic cavitation is ignored to promote the dissolution of sugar beet meal; 3) The insufficient utilization of secondary waste meal after sugar beet pectin extraction leads to the waste of resources; 4 ) Cellulose used in Pickering emulsification requires a tedious separation and purification process and must be repeatedly modified or compounded with other substances to have good Pickering emulsification. This process requires the use of a large amount of acids, bases, strong oxidants and enzyme preparations, which is costly. High and environmentally unfriendly; 5) Beet pectin emulsification stability is poor; 6) The synergistic emulsification effect between fiber Pickering emulsifier and soluble components is ignored.
技术解决方案Technical solutions
本发明旨在拓展甜菜粕的应用领域，提供一种食品级的方法将甜菜粕的全组分转化为乳化增稠剂的甜菜粕全组分乳化增稠剂及其制备方法，实现甜菜粕资源的全利用。The present invention aims to expand the application field of beet pulp, provide a food-grade method to convert all components of beet pulp into an emulsifying thickening agent, and a preparation method thereof to achieve Full utilization of sugar beet meal resources.
本发明另一目的在于提供所述的甜菜粕全组分乳化增稠剂对含脂酱料、奶油或酸奶乳化增稠的应用。Another object of the present invention is to provide the application of the whole-component emulsifying thickener of beet pulp for emulsifying and thickening fat-containing sauces, cream or yogurt.
本发明的目的通过如下技术方案实现：The object of the present invention is achieved through the following technical solutions:
一种甜菜粕全组分乳化增稠剂的制备方法，包括如下步骤：A method for preparing a full-component emulsifying thickener of beet pulp, including the following steps:
1）清洗粉碎预处理； 1) Cleaning and crushing pretreatment;
2）取清洗粉碎预处理后的甜菜粕粉末分散于水中，置于高压反应釜中控制温度为110~140℃水热处理0.5~4 h；2) Disperse the cleaned, crushed and pre-treated sugar beet meal powder in water, place it in a high-pressure reactor and control the temperature to 110~140°C for hydrothermal treatment for 0.5~4 hours;
3）向步骤2）获得的水热处理甜菜粕分散液中加水稀释后搅拌的同时进行高能超声破碎处理；3) Add water to dilute the hydrothermally treated beet pulp dispersion obtained in step 2) and perform high-energy ultrasonic crushing while stirring;
4）对步骤3）获得的超声破碎甜菜粕分散液进行浓缩后干燥，获得甜菜粕全组分乳化增稠剂。4) Concentrate and then dry the ultrasonic crushed beet pulp dispersion obtained in step 3) to obtain a full-component emulsifying thickener of sugar beet pulp.
为进一步实现本发明目的，优选地，所述的清洗粉碎预处理是将甜菜压粕在水中浸泡直至甜菜丝吸水发胀分散，去除其中包括泥土木屑在内的杂质及焦黑甜菜丝，再将甜菜粕从水中捞出除去部分水分后烘干，将干燥甜菜粕粉碎过筛后置于阴凉处备用。In order to further realize the object of the present invention, preferably, the cleaning and grinding pretreatment is to soak the pressed beet pulp in water until the beet shreds absorb water, swell and disperse, remove impurities including soil and sawdust and burnt beet shreds, and then sweeten the sugar beet shreds. The rapeseed meal is taken out of the water, part of the water is removed, and then dried. The dried beet pulp is crushed and sieved and placed in a cool place for later use.
优选地，所述的除去部分水是采用螺旋挤压机进行；所述的烘干是在烘箱进行；控制烘干的温度为45~65 ℃，时间为10~24 h，甜菜粕干燥后的水分含量为6wt%~9wt%。Preferably, the removal of part of the water is carried out using a screw extruder; the drying is carried out in an oven; the drying temperature is controlled to be 45~65°C and the time is 10~24 h. After the sugar beet pulp is dried, The moisture content is 6wt%~9wt%.
优选地，干燥甜菜粕粉碎过筛的筛网目数为100~400目。Preferably, the mesh size of the crushed and sieved dried sugar beet pulp is 100 to 400 mesh.
优选地，所述的清洗粉碎预处理后的甜菜粕粉末分散于水中所形成的甜菜粕悬液浓度为2wt%~20wt%。Preferably, the concentration of the sugar beet pulp suspension formed by dispersing the washed, crushed and pretreated sugar beet pulp powder in water is 2wt%~20wt%.
优选地，所述的水热处理温度为120~130℃，时间为1-1.5 h。Preferably, the hydrothermal treatment temperature is 120~130°C and the time is 1-1.5 h.
优选地，加水稀释后的水热处理甜菜粕分散液的浓度为0.5wt%~5wt%；所述的高能超声破碎处理的功率密度为127~255 W/cm 2，时间为5~25 min；所采用的高能超声破碎处理模式为持续2 s，间隔2 s，处理过程中水热处理甜菜粕分散液采用200～600rpm转速机械搅拌，搅拌在敞口容器中进行，以便向体系中混入少量气泡，且以-4~4℃循环冰水浴进行冷却使体系温度不高于45℃。 Preferably, the concentration of the hydrothermally treated beet pulp dispersion diluted with water is 0.5wt%~5wt%; the power density of the high-energy ultrasonic crushing treatment is 127~255 W/cm 2 and the time is 5~25 min; The high-energy ultrasonic crushing treatment mode used is 2 s continuous and 2 s intervals. During the treatment process, the hydrothermal treatment beet pulp dispersion is mechanically stirred at a speed of 200 to 600 rpm. The stirring is carried out in an open container to mix a small amount of air bubbles into the system. , and use a -4~4°C circulating ice water bath to cool the system so that the system temperature is not higher than 45°C.
优选地，所述的浓缩的方式采用减压浓缩或超滤膜过滤浓缩；当浓缩至13wt%~15wt%时采用喷雾干燥的方法进行干燥。Preferably, the concentration method adopts reduced pressure concentration or ultrafiltration membrane filtration and concentration; when concentrated to 13wt%~15wt%, spray drying is used for drying.
一种甜菜粕全组分乳化增稠剂，由上述的制备方法制得，所得甜菜粕全组分乳化增稠剂的可溶性组分含量为39.5wt%~45.1wt%，可溶性果胶含量为24.3wt%~29.7wt%，可溶果胶的分子量为392~561kDa，并含有香味，纤维是直径为50~200 nm，长度为3~50 μm的条状纳米纤维丝。A kind of beet pulp full-component emulsification thickener, prepared by the above preparation method. The soluble component content of the obtained sugar beet pulp whole-component emulsification thickener is 39.5wt%~45.1wt%, and the soluble pectin content It is 24.3wt%~29.7wt%. The molecular weight of soluble pectin is 392~561kDa and contains fragrance. The fiber is a strip-shaped nanofiber filament with a diameter of 50~200 nm and a length of 3~50 μm.
所述的甜菜粕全组分乳化增稠剂对含脂酱料、奶油或酸奶乳化增稠的应用；甜菜粕全组分乳化增稠剂在用于乳化增稠前进行充分的分散和水化。The application of the whole-component emulsifying thickener of beet pulp to the emulsification and thickening of fat-containing sauces, cream or yogurt; the whole-component emulsifying thickener of beet pulp is fully dispersed and thickened before being used for emulsification and thickening. Hydration.
有益效果beneficial effects
本发明与现有技术相比具有如下优点：Compared with the prior art, the present invention has the following advantages:
1）本发明主要对甜菜粕进行水热处理，再进行搅拌高能超声破碎处理，将致密的甜菜粕纤维解离成不溶性纳米纤维丝及可溶性大分子甜菜果胶组分。该方法减少了甜菜果胶在溶出过程中的降解，保护了其所具有的可溶性胶体乳化性；同时促进了纳米纤维丝的解离，增强其作为不溶固体的皮克林乳化性。1) The present invention mainly performs hydrothermal treatment on sugar beet pulp, and then performs stirring and high-energy ultrasonic crushing treatment to dissociate the dense sugar beet pulp fibers into insoluble nanofibers and soluble macromolecular sugar beet pectin components. This method reduces the degradation of sugar beet pectin during the dissolution process and protects its soluble colloidal emulsification properties; at the same time, it promotes the dissociation of nanofibers and enhances its Pickering emulsification properties as an insoluble solid.
2）本发明采用水热软化致密细胞壁，搅拌强化超声空化剥离果胶的方法获取降解程度低的甜菜果胶，保护其大分子结构及两亲性。2) The present invention uses hydrothermal softening of dense cell walls and stirring to enhance ultrasonic cavitation to peel off pectin to obtain sugar beet pectin with a low degree of degradation and protect its macromolecular structure and amphiphilicity.
3）本发明将可溶果胶和不溶性纳米纤维丝共同作为全组分乳化增稠剂，无需分离，实现甜菜粕百分百利用。3) The present invention uses soluble pectin and insoluble nanofibers together as a full-component emulsification thickener without separation, realizing 100% utilization of sugar beet pulp.
4）本发明所得纳米纤维丝无需深度分离纯化或进一步改性复合，且具有皮克林乳化作用，过程无需酸碱强氧化剂及酶，绿色且环境友好。4) The nanofiber silk obtained by the present invention does not require deep separation, purification or further modification and compounding, and has Pickering emulsification effect. The process does not require acid and alkali strong oxidants and enzymes, and is green and environmentally friendly.
5）本发明纳米纤维丝可与甜菜果胶发挥协同乳化作用，纳米纤维丝具有弯曲柔韧性可贴合在油滴表面，形成交错的纤维网状吸附层，其空隙被具有表面活性的果胶所覆盖，两者共同吸附带油水界面上，在油水界面形成紧密的界面膜，不溶性纳米纤维丝的空间屏障效应显著阻止油滴间相互接触，克服甜菜果胶的乳化稳定性差的问题。5) The nanofiber silk of the present invention can exert a synergistic emulsification effect with sugar beet pectin. The nanofiber silk has bending flexibility and can fit on the surface of oil droplets to form a staggered fiber network adsorption layer, and its gaps are filled with surface-active pectin. Covered, the two co-adsorb at the oil-water interface, forming a tight interfacial film at the oil-water interface. The spatial barrier effect of the insoluble nanofibers significantly prevents oil droplets from contacting each other, overcoming the problem of poor emulsification stability of sugar beet pectin.
6）本发明采用水热-超声处理对甜菜粕细胞壁中含量丰富且乳化活性良好的果胶质进行剥离的同时将甜菜纤维组分解离为具有皮克林乳化性的纳米纤维丝，避免酸碱强氧化剂的使用，环境友好。6) The present invention uses hydrothermal-ultrasonic treatment to peel off pectin, which is rich in content and has good emulsifying activity in the cell wall of beet pulp, and at the same time separates the beet fiber component into nanofiber filaments with Pickering emulsification properties to avoid acid The use of strong alkali oxidants is environmentally friendly.
7）本发明采用高能超声破碎技术，在可溶多糖/不溶纤维混合体系中保护甜菜果胶大分子结构；无需深度提取纯化纤维素，将具有协同乳化作用的可溶性果胶和纤维素纳米丝同作为甜菜粕全组分应用于乳化增稠剂，克服甜菜果胶乳化稳定性差的问题，实现甜菜粕全利用。7) The present invention uses high-energy ultrasonic crushing technology to protect the macromolecular structure of beet pectin in the soluble polysaccharide/insoluble fiber mixed system; without the need for deep extraction and purification of cellulose, the soluble pectin and cellulose nanofilaments with synergistic emulsification effect are combined at the same time. As a complete component of sugar beet meal, it is used as an emulsification thickener to overcome the problem of poor emulsification stability of sugar beet pectin and achieve full utilization of sugar beet meal.
8）本发明采用一锅法操作，工艺简单且分离纯化操作少，无需额外添加化学试剂，绿色无毒，产品使用方是法简单，可应用于食品产业。8) The present invention adopts a one-pot method, which has a simple process and few separation and purification operations. No additional chemical reagents are needed. It is green and non-toxic. The product usage method is simple and can be applied to the food industry.
附图说明Description of the drawings
图1为本发明应用的高能超声处理设备示意图。Figure 1 is a schematic diagram of the high-energy ultrasonic treatment equipment used in the present invention.
图2为实施例1所得产品的不溶性纤维的原子显微镜图。Figure 2 is an atomic microscope image of the insoluble fiber of the product obtained in Example 1.
图3为实施例1中原始甜菜粕的光学显微镜图。Figure 3 is an optical microscope picture of the original sugar beet pulp in Example 1.
图4为实施例1的产品悬浮液外观图和原始甜菜粕粉末悬浮液外观图。Figure 4 shows the appearance of the product suspension and the original sugar beet pulp powder suspension in Example 1.
图5为实施例1产品制备的乳液光学显微镜图。Figure 5 is an optical microscope picture of the emulsion prepared from the product of Example 1.
图6为对比例1制备的乳液的光学显微镜图。Figure 6 is an optical microscope image of the emulsion prepared in Comparative Example 1.
图7为实施例1产品制备的乳液(a)和对比例1制备的乳液(b)的乳化机理图。Figure 7 is a diagram of the emulsification mechanism of the emulsion (a) prepared by the product of Example 1 and the emulsion (b) prepared by Comparative Example 1.
图8为对比例1所得产品的不溶性颗粒的光学显微镜图。Figure 8 is an optical microscope image of insoluble particles of the product obtained in Comparative Example 1.
图9为对比例1的产品悬浮液外观图(a)和原始甜菜粕粉末悬浮液外观图(b)。Figure 9 shows the appearance of the product suspension of Comparative Example 1 (a) and the appearance of the original sugar beet pulp powder suspension (b).
本发明的实施方式Embodiments of the invention
为进一步理解本发明，下面结合附图和实施例对本发明进行进一步阐述，但本发明的实施方式不限于此，还可以有许多变形。In order to further understand the present invention, the present invention will be further described below in conjunction with the drawings and examples. However, the implementation of the present invention is not limited thereto, and many modifications are possible.
本发明先对甜菜粕进行水热处理，再进行搅拌高能超声破碎处理，甜菜粕富含乳化性良好的果胶组分，经过水热处理后，共价结合在细胞壁的化合物发生化学键的断裂，果胶及半纤维素组分溶出，使原本致密的细胞壁组织结构变得多孔松散，发生溶胀且比表面积增大。大比表面积的粗糙表面能够降低超声的空化阈，为高能超声（127-255 W/cm 2）过程提供更多的空化气泡起核位点，能够在粗糙的多孔甜菜粕表面及内部生成大量的空化气泡而冲击甜菜粕使其解离为直径为纳米级别而长达数十微米的纤维细丝。本发明体系中混合有溶解果胶与不溶性甜菜粕颗粒（总浓度为0.5wt%-5wt%），多孔的甜菜粕不仅促进超声空化过程，还吸收了大部分的超声能量，已溶解的大分子甜菜果胶因未吸收足够超声能量得到保护而没有发生显著降解。如图1所示，超声过程的机械搅拌（200-600 rpm）向体系中混入少量空气，使得超声空化气泡可以源源不断补充生成。水热预处理及搅拌高能超声处理在甜菜粕的破碎过程中发挥着协同作用，不仅可以促使大分子果胶组分溶出，保护其结构不被降解而发挥良好的乳化性能，同时可以强化高能超声的空化效应，使多孔甜菜粕解离为纳米纤维丝而形成胶体稳定性好且能发挥良好的皮克林稳定效应。在不进行进一步分离的情况下，高长径比的纳米纤维素和大分子果胶共同吸附到水油界面上，发挥着乳化稳定效应，可以制备出粒径更小且不易分层的稳定乳液，克服天才果胶乳化稳定性差的问题。 In the present invention, beet pulp is first subjected to hydrothermal treatment, and then subjected to stirring and high-energy ultrasonic crushing treatment. The beet pulp is rich in pectin components with good emulsification properties. After hydrothermal treatment, the chemical bonds of the compounds covalently bound to the cell wall are broken. The pectin and hemicellulose components dissolve, causing the originally dense cell wall tissue structure to become porous and loose, causing swelling and an increase in the specific surface area. A rough surface with a large specific surface area can reduce the cavitation threshold of ultrasound, provide more cavitation bubble nucleation sites for the high-energy ultrasound (127-255 W/cm 2 ) process, and can achieve the desired effect on the surface and interior of rough porous sugar beet pulp. A large number of cavitation bubbles are generated and impact the beet pulp to dissociate it into fiber filaments with a diameter of nanometer level and a length of tens of microns. The system of the present invention is mixed with dissolved pectin and insoluble sugar beet pulp particles (total concentration is 0.5wt%-5wt%). The porous sugar beet pulp not only promotes the ultrasonic cavitation process, but also absorbs most of the ultrasonic energy and has been dissolved. The macromolecular sugar beet pectin was protected from significant degradation because it did not absorb enough ultrasound energy. As shown in Figure 1, the mechanical stirring (200-600 rpm) of the ultrasonic process mixes a small amount of air into the system, so that ultrasonic cavitation bubbles can be continuously replenished and generated. Hydrothermal pretreatment and stirring high-energy ultrasonic treatment play a synergistic role in the crushing process of sugar beet pulp. They can not only promote the dissolution of macromolecular pectin components, protect their structure from degradation and exert good emulsification properties, but also strengthen the high-energy The cavitation effect of ultrasound dissociates porous beet pulp into nanofibers to form a colloid with good colloidal stability and can exert a good Pickering stabilization effect. Without further separation, high aspect ratio nanocellulose and macromolecular pectin are jointly adsorbed to the water-oil interface, exerting an emulsification stabilizing effect, and can prepare stable emulsions with smaller particle sizes and less likely to stratify. , to overcome the problem of poor emulsification stability of genius pectin.
相比之下，不经过水热处理而直接进行超声处理，果胶及半纤维素与纤维素共价结合的交联结构使得细胞壁结构紧密而阻碍破碎，甜菜粕颗粒不能被解离成纳米丝且维持原有的颗粒状态，会因重力作用快速沉降而不能形成稳定胶体悬浮液。单纯的水热处理而没有后续的高能超声处理只能使甜菜粕发生溶胀而不能破碎甜菜粕颗粒。In contrast, when ultrasonic treatment is performed directly without hydrothermal treatment, the cross-linked structure of pectin and hemicellulose covalently bonded to cellulose makes the cell wall structure tight and hinders breakage, and the sugar beet pulp particles cannot be dissociated into nanofilaments. And if it maintains its original particle state, it will rapidly settle due to gravity and cannot form a stable colloidal suspension. Simple hydrothermal treatment without subsequent high-energy ultrasonic treatment can only cause the sugar beet pulp to swell but cannot break the sugar beet pulp particles.
本发明的实施例及附图所涉及的数据，有关的检测方法说明如下：The data involved in the embodiments of the present invention and the accompanying drawings, and the relevant detection methods are described as follows:
（1）产品中可溶物比例及组分含量的测定(1) Determination of the proportion of soluble matter and component content in the product
将产品分散于水中制备浓度为3wt%的悬液，采用高速剪切仪在20000 rpm转速下分散5 min，随后进行机械搅拌5 h使其充分分散。悬浊液在10000 g离心力下离心30 min，取上清液。上清液冻干后对干燥的可溶性进行称重，可溶物总量占原产品干重的比例则为可溶物比例。取冻干后的可溶物进行凯氏定氮实验，测定可溶物中的蛋白质含量，蛋白质转换系数为6.25。蛋白质总量占原产品干重的比例则为可溶性蛋白的含量。取3倍体积95%乙醇溶液与1倍体积上清液中进行果胶醇析，析出的果胶进行离心，在45℃下烘干至恒重，所得即为粗果胶，采用开始定氮法测定果胶中的蛋白质含量。粗果胶占原产品干重的比例则为可溶果胶含量。Disperse the product in water to prepare a suspension with a concentration of 3wt%, use a high-speed shear instrument to disperse at 20,000 rpm for 5 minutes, and then mechanically stir for 5 hours to fully disperse. The suspension was centrifuged at 10,000 g for 30 min, take the supernatant. After the supernatant is freeze-dried, the dried soluble content is weighed. The ratio of the total soluble content to the dry weight of the original product is the soluble content ratio. Take the freeze-dried solubles and perform a Kjeldahl nitrogen test to determine the protein content in the solubles. The protein conversion coefficient is 6.25. The ratio of the total protein to the dry weight of the original product is the soluble protein content. Take 3 times the volume of 95% ethanol solution and 1 times the volume of the supernatant to perform alcohol precipitation of pectin. The precipitated pectin is centrifuged and dried at 45°C to constant weight. The result is crude pectin. Use the initial nitrogen determination method. method to determine the protein content in pectin. The proportion of crude pectin to the dry weight of the original product is the soluble pectin content.
（2）果胶分子量的测定(2) Determination of pectin molecular weight
采用高效液相-体积排阻色谱法测定甜菜果胶分子量，色谱柱为Ultrahydrogel Guard，Ultrahydrogel 2000和Ultrahydrogel 1000三柱连用，采用折光示差检测器检测，流动相为0.1 mol/L硝酸钠溶液（包含0.05wt%叠氮化钠），流速为0.6 mL/min，温度35 ℃，进样量100 μL。采用分子量为4400~667000 Da的葡聚糖标准品做标准曲线进行相对分子量定量。High performance liquid chromatography-size exclusion chromatography was used to determine the molecular weight of sugar beet pectin. The chromatographic column was Ultrahydrogel. Guard, Ultrahydrogel 2000 and Ultrahydrogel 1000 are used together with three columns, using a refractive index detector, and the mobile phase is 0.1 mol/L sodium nitrate solution (containing 0.05wt% sodium azide), flow rate is 0.6 mL/min, temperature 35°C, injection volume 100 μL. Dextran standards with molecular weights of 4400 to 667000 Da were used as standard curves for relative molecular weight quantification.
（3）产品表观粘度的测定(3) Determination of product apparent viscosity
产品悬浊液的表观粘度测定采用配有40mm直径平板转子的TA旋转流变仪测定。测定条件10/s，温度为25℃。The apparent viscosity of the product suspension was measured using a TA rotational rheometer equipped with a 40mm diameter flat plate rotor. The measurement conditions are 10/s and the temperature is 25°C.
（4）不溶性纳米纤维丝的形貌观察(4) Observation of morphology of insoluble nanofibers
取充分分散的浓度为1wt%的产品在10000 g离心力下离心30min，倒去上清液。加水至沉淀中到原体积，并使用高速剪切仪在20000 rpm转速下分散5 min，随后进行机械搅拌5h使其充分分散。取分散液加水稀释500倍体积后，采用原子力显微镜在轻敲模式下观察形貌。Take the fully dispersed product with a concentration of 1wt%, centrifuge it at 10,000g for 30 minutes, and pour off the supernatant. Add water to the precipitate to its original volume, and use a high-speed shear instrument at 20,000 Disperse at rpm for 5 minutes, then mechanically stir for 5 hours to fully disperse. After diluting the dispersion 500 times with water, the morphology was observed using an atomic force microscope in tapping mode.
（5）乳液的制备及粒径测定(5) Preparation of emulsion and determination of particle size
将甜菜粕全组分乳化增稠剂悬液的pH调节为7，向270 g充分分散的甜菜粕全组分乳化增稠剂悬液中加入30 g玉米油，采用高速剪切仪在20000 rpm转速下分散2 min进行预均质制备粗乳液，而后采用高压均质机在50 MPa压力下循环均质两次得到水包油乳液。Adjust the pH of the beet meal full-component emulsified thickener suspension to 7, add 30 g of corn oil to 270 g of the fully dispersed beet meal full-component emulsified thickener suspension, and use a high-speed shear to Disperse for 2 minutes at 20,000 rpm for pre-homogenization to prepare a coarse emulsion, and then use a high-pressure homogenizer to circulate and homogenize twice under a pressure of 50 MPa to obtain an oil-in-water emulsion.
乳液粒径 d 4,3的测定采用马尔文MS3000激光粒度仪测定。以水为分散介质，测定新鲜制备乳液的粒径以及常温下密封放置60天的乳液粒径。乳液粒径 d 4,3的变化越大则代表乳化稳定性越差。 The emulsion particle size d 4,3 was measured using a Malvern MS3000 laser particle size analyzer. Using water as the dispersion medium, measure the particle size of freshly prepared emulsion and the particle size of emulsion that has been sealed and stored at room temperature for 60 days. The greater the change in emulsion particle size d 4,3 , the worse the emulsion stability.
实施例1 Example 1
制备：选取1 kg来自新疆的甜菜压粕浸泡于10 L自来水中，直至压粕吸水胀大分散成条状的甜菜粕，将少部分石头、木头、铁丝等在内的杂质以及部分成焦黑状的甜菜丝去除，将悬浮在水中的甜菜粕捞出并采用螺旋挤压机压去大部分水分，直至甜菜粕表面没有明显滴水。所得甜菜粕置于烘箱中烘干，温度为65℃，时间为10 h，烘干过程中人工翻动数次以防止微生物繁殖发酵。随后采用高速粉碎机粉碎过100目筛备用。取甜菜粕粉末分散于水形成浓度约为20wt%的甜菜粕悬液，置于高压反应釜中以110~120 ℃处理4 h。Preparation: Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 65°C for 10 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation. Then use a high-speed pulverizer to crush it and pass it through a 100-mesh sieve for later use. Take the beet pulp powder and disperse it in water to form a sugar beet pulp suspension with a concentration of about 20wt%. Place it in a high-pressure reaction kettle at 110~120 ℃ treatment for 4 h.
如图1所示，所得甜菜粕悬液冷却至常温后加水稀释甜菜浆浓度约为5wt%，总体积为5 L采用探头式高能超声法对甜菜粕进行破碎处理，超声功率127 W/cm 2，处理时间30 min，超声持续时间2 s，间隔2 s，该过程中采用600 rpm转速机械搅拌向体系中混入少量气泡使体系被超声均匀处理且以冰水浴进行冷却使悬浊液在处理过程中温度不超过45 ℃。所得粘稠悬浊液可采用膜浓缩或减压浓缩至浓度为13wt%~15wt%后进行喷雾干燥得实施例1甜菜粕全组分乳化增稠剂。 As shown in Figure 1, the obtained sugar beet pulp suspension is cooled to normal temperature and then water is added to dilute the sugar beet pulp to a concentration of about 5wt%. The total volume is 5 L. The probe-type high-energy ultrasonic method is used to crush the sugar beet pulp. The ultrasonic power is 127 W/ cm 2 , treatment time 30 min, ultrasonic duration 2 s, interval 2 s. During the process, mechanical stirring at 600 rpm was used to mix a small amount of bubbles into the system so that the system was evenly treated by ultrasonic and cooled with an ice-water bath to make the suspension in The temperature during processing should not exceed 45°C. The obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt%~15wt% and then spray-dried to obtain the beet pulp full-component emulsifying thickener of Example 1.
使用：实施例1产品粉末分散于水中形成浓度为5wt%的悬液，采用高速剪切均质的方法对悬液进行均质，转速为19000~20000 rpm，均质时间为8 min，而后采用机械搅拌的方式在450~500 rpm转速下搅拌15 h。所得悬液可稀释后或直接用于乳化增稠；如本实施例全组分乳化增稠剂适用于沙拉酱/蛋黄酱的制备。相比于传统的蛋黄卵磷脂乳化剂，本施例全组分乳化增稠剂可大幅增加酱料中膳食纤维的含量，并通过形成空间网络结构增加酱料的粘稠度以及乳液的稳定性，延缓油脂的消化和降低油脂的消化率，以实现减油的目标。所得全组分乳化增稠剂还可应用于奶油搅打中，本产品相比于常见的单/双甘油脂肪酸酯，能制备出塑性更好的奶油产品，本实施例全组分乳化增稠剂所形成的纤维网络结构使得乳液稳定性更持久。Usage: The product powder of Example 1 is dispersed in water to form a suspension with a concentration of 5wt%. The suspension is homogenized using high-speed shear homogenization method. The rotation speed is 19000~20000 rpm. The homogenization time is 8 minutes. Then use Mechanical stirring was performed at 450~500 rpm for 15 h. The obtained suspension can be diluted or directly used for emulsification and thickening; for example, the full-component emulsification thickener in this embodiment is suitable for the preparation of salad dressing/mayonnaise. Compared with the traditional egg yolk lecithin emulsifier, the full-component emulsifying thickener of this embodiment can significantly increase the content of dietary fiber in the sauce, and increase the viscosity of the sauce and the stability of the emulsion by forming a spatial network structure. , delaying the digestion of oil and reducing the digestibility of oil to achieve the goal of reducing oil. The obtained full-component emulsifying thickener can also be used in cream whipping. Compared with common mono/diglycerol fatty acid esters, this product can prepare cream products with better plasticity. In this embodiment, the full-component emulsifying thickener The fiber network structure formed by the thickener makes the emulsion more stable.
本实施例1所制备的甜菜粕全组分乳化剂可溶性固形物比例为39.5wt%，其中可溶性果胶组分含量为24.3wt%，可溶性果胶的分子量为561 kDa，如表1所示。不溶性组分解离为直径为50~200 nm，长度为3~50 μm不等的纳米纤维丝（如图2原子力显微镜照片所示）。所得产品在0.5wt%的浓度下外观为均匀不分层的纤维胶体絮状物（图3），胶体稳定性良好，而原始甜菜粕分层明显且几乎不发生溶胀（图4中b，图4中a为实施例1的产品悬浮液外观图），其光学显微镜照显示其为直径达十几至几十微米的、表面具有规则边缘的块状颗粒（图3）；0.5wt%的本实施例产品的表观粘度1.153 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.022 Pa·s，本实施例产品具有良好的增稠性。0.5wt%浓度下的本实施例产品可制备20wt%的玉米油乳液，其乳液粒径 d 4,3为6.24 μm，乳液在室温下存放60天乳液粒径 d 4,3为6.31 μm，乳液没有发生明显乳析分层现象，乳化稳定性良好。本实施例产品制备的乳液的显微镜照片显示其表面光滑（图5），直径为纳米级的纤维细丝在界面上为透明状而不可直接观测，其乳液形成机理如图7中a所示，纳米纤维丝交错形成网状结构贴合吸附在乳液界面，而空隙被可溶性果胶所覆盖，形成紧密的网络界面膜结构，协同维持乳液稳定。作为对照的甜菜果胶在0.5wt%浓度下单独制备20wt%的玉米油乳液，其乳液粒径 d 4,3为1.16 μm，乳液在室温下存放60天乳液粒径 d 4,3为35.2 μm，乳液出现明显乳析分层，乳化稳定性较差。 The soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in Example 1 is 39.5wt%, of which the soluble pectin component content is 24.3wt%, and the molecular weight of the soluble pectin is 561 kDa, as shown in Table 1 . The insoluble components dissociate into nanofiber filaments with diameters of 50 to 200 nm and lengths of 3 to 50 μm (as shown in the atomic force microscope photo in Figure 2). At a concentration of 0.5wt%, the obtained product appears as uniform and non-stratified fibrous colloid floc (Figure 3), with good colloid stability, while the original sugar beet pulp has obvious stratification and almost no swelling (b, Figure 4) a in Figure 4 is the appearance of the product suspension of Example 1), and its optical microscope photo shows that it is massive particles with a diameter of more than ten to tens of microns and regular edges on the surface (Figure 3); 0.5wt% The apparent viscosity of the product in this example is 1.153 Pa·s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa·s and 0.022 Pa·s. The product in this example has good thickening sex. The product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion. The emulsion particle size d 4,3 is 6.24 μm. When the emulsion is stored at room temperature for 60 days, the emulsion particle size d 4,3 is 6.31 μm. No obvious emulsion stratification occurred, and the emulsification stability was good. The micrograph of the emulsion prepared by the product of this example shows that its surface is smooth (Figure 5). The fiber filaments with a diameter of nanometers are transparent at the interface and cannot be directly observed. The formation mechanism of the emulsion is shown in a in Figure 7. The nanofiber filaments are interlaced to form a network structure that adheres to the emulsion interface, and the gaps are covered by soluble pectin, forming a tight network interface film structure, which synergistically maintains the stability of the emulsion. As a control, a 20wt% corn oil emulsion of beet pectin was prepared separately at a concentration of 0.5wt%. The emulsion particle size d 4,3 was 1.16 μm. The emulsion particle size d 4,3 was 35.2 μm after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
实施例2Example 2
制备：选取1 kg来自新疆的甜菜压粕浸泡于10 L自来水中，直至压粕吸水胀大分散成条状的甜菜粕，将少部分石头、木头、铁丝等在内的杂质以及部分成焦黑状的甜菜丝去除，将悬浮在水中的甜菜粕捞出并采用螺旋挤压机压去大部分水分，直至甜菜粕表面没有明显滴水。所得甜菜粕置于烘箱中烘干，温度为45℃，时间为24 h，烘干过程中人工翻动数次以防止微生物繁殖发酵。随后采用高速粉碎机粉碎过400目筛备用。取甜菜粕粉末分散于水形成浓度约为2wt%的甜菜粕悬液，置于高压反应釜中以130~140 ℃处理0.5 h。所得甜菜粕悬液冷却至常温后加水稀释甜菜浆浓度约为0.5wt%，总体积为2L，采用探头式高能超声法对甜菜粕进行破碎处理。超声功率255 W/cm 2，处理时间5 min，超声持续时间2 s，间隔2 s，该过程中采用200 rpm转速机械搅拌向体系中混入少量气泡使体系被超声均匀处理且以冰水浴进行冷却使悬浊液在处理过程中温度不超过45 ℃。所得粘稠悬浊液可采用膜浓缩或减压浓缩至浓度为13wt%~15wt%后进行喷雾干燥得甜菜粕全组分乳化增稠剂。 Preparation: Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 45°C for 24 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation. Then use a high-speed pulverizer to crush it and pass it through a 400-mesh sieve for later use. Disperse the sugar beet pulp powder in water to form a sugar beet pulp suspension with a concentration of approximately 2wt%, and place it in a high-pressure reaction kettle for treatment at 130~140°C for 0.5 h. The obtained sugar beet pulp suspension is cooled to normal temperature and then water is added to dilute the sugar beet pulp to a concentration of approximately 0.5wt%. The total volume is 2L. The probe-type high-energy ultrasonic method is used to crush the sugar beet pulp. The ultrasonic power is 255 W/cm 2 , the treatment time is 5 min, the ultrasonic duration is 2 s, and the interval is 2 s. In the process, mechanical stirring at 200 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath. The temperature of the suspension should not exceed 45°C during treatment. The obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt%~15wt% and then spray-dried to obtain a full-component emulsified thickening agent for sugar beet pulp.
使用：产品粉末分散于水中形成浓度为0.8wt%的悬液，采用高速剪切均质的方法对悬液进行均质，转速为19000~20000 rpm，均质时间为2 min，而后采用机械搅拌的方式在450~500 rpm转速下搅拌5 h。所得悬液可稀释后或直接用于乳化增稠。Usage: The product powder is dispersed in water to form a suspension with a concentration of 0.8wt%. The suspension is homogenized using high-speed shear homogenization method with a rotation speed of 19000~20000. rpm, the homogenization time is 2 minutes, and then mechanical stirring is used at 450~500 Stir at rpm for 5 h. The resulting suspension can be diluted or directly used for emulsification and thickening.
本实施例所制备的甜菜粕全组分乳化剂可溶性固形物比例为45.1wt%，其中可溶性果胶组分含量为29.7wt%，可溶性果胶的分子量为392 kDa，如表1所示。不溶性组分解离为直径为50~200 nm，长度为3~50 μm不等的纳米纤维丝。所得产品在0.5wt%的浓度下外观为均匀不分层的纤维胶体絮状物，胶体稳定性良好，而原始甜菜粕分层明显且几乎不发生溶胀，呈块状结构；0.5wt%的本实施例产品的表观粘度1.361 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.019 Pa·s，本实施例产品具有良好的增稠性。0.5wt%浓度下的本实施例产品可制备20wt%的玉米油乳液，其乳液粒径 d 4,3为5.73 μm，乳液在室温下存放60天乳液粒径 d 4,3为5.80 μm，乳液没有发生明显乳析分层现象，乳化稳定性良好。作为对照的甜菜果胶在0.5wt%浓度下单独制备20wt%的玉米油乳液，其乳液粒径 d 4,3为1.36 μm，乳液在室温下存放60天乳液粒径 d 4,3为28.8 μm，乳液出现明显乳析分层，乳化稳定性较差。 The soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in this example is 45.1wt%, of which the soluble pectin component content is 29.7wt%, and the molecular weight of the soluble pectin is 392 kDa, as shown in Table 1. The insoluble components are dissociated into nanofibers with diameters of 50 to 200 nm and lengths of 3 to 50 μm. At a concentration of 0.5wt%, the obtained product appears as a uniform non-stratified fibrous colloid floc with good colloid stability, while the original sugar beet pulp is obviously stratified and almost does not swell, showing a massive structure; 0.5wt% The apparent viscosity of the product in this example is 1.361 Pa·s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa·s and 0.019 Pa·s. The product in this example has good thickening sex. The product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion. The emulsion particle size d 4,3 is 5.73 μm. When the emulsion is stored at room temperature for 60 days, the emulsion particle size d 4,3 is 5.80 μm. No obvious emulsion stratification occurred, and the emulsification stability was good. As a control, a 20wt% corn oil emulsion of beet pectin was prepared separately at a concentration of 0.5wt%. The emulsion particle size d 4,3 was 1.36 μm. The emulsion particle size d 4,3 was 28.8 μm after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
实施例3：Example 3:
制备：选取1 kg来自新疆的甜菜压粕浸泡于10 L自来水中，直至压粕吸水胀大分散成条状的甜菜粕，将少部分石头、木头、铁丝等在内的杂质以及部分成焦黑状的甜菜丝去除，将悬浮在水中的甜菜粕捞出并采用螺旋挤压机压去大部分水分，直至甜菜粕表面没有明显滴水。所得甜菜粕置于烘箱中烘干，温度为55℃，时间为15 h，烘干过程中人工翻动数次以防止微生物繁殖发酵。随后采用高速粉碎机将干粕粉碎后过200目筛备用。取甜菜粕粉末分散于水形成浓度约为10wt%的甜菜粕悬液，置于高反应釜中以120~130 ℃处理1.5 h。所得甜菜粕悬液冷却至常温后加水稀释甜菜浆浓度约为2.5wt%，总体积为4 L，采用探头式高能超声法对甜菜粕进行破碎处理。超声功率190 W/cm 2，处理时间12 min，超声持续时间2 s，间隔2 s，该过程中采用400 rpm转速机械搅拌向体系中混入少量气泡使体系被超声均匀处理且以冰水浴进行冷却使悬浊液在处理过程中温度不超过45 ℃。所得粘稠悬浊液可采用膜浓缩或减压浓缩至浓度为13wt%~15wt%后进行喷雾干燥得甜菜粕全组分乳化增稠剂。 Preparation: Select 1 kg of pressed sugar beet meal from Xinjiang and soak it in 10 L of tap water until the pressed meal absorbs water and swells and disperses into strips of sugar beet meal. Remove a small amount of impurities such as stones, wood, wires, etc. and burn them black. Remove the beet-shaped shreds, take out the beet pulp suspended in the water, and use a screw extruder to press out most of the water until there is no obvious dripping water on the surface of the beet pulp. The obtained sugar beet pulp was dried in an oven at a temperature of 55°C for 15 h. During the drying process, it was manually turned several times to prevent microbial reproduction and fermentation. Then use a high-speed pulverizer to crush the dry meal and pass it through a 200-mesh sieve for later use. Disperse the sugar beet pulp powder in water to form a sugar beet pulp suspension with a concentration of approximately 10wt%, and place it in a high-pressure reaction kettle for treatment at 120~130°C for 1.5 hours. The obtained sugar beet pulp suspension was cooled to normal temperature and then water was added to dilute the sugar beet pulp to a concentration of approximately 2.5wt%. The total volume was 4 L. The probe-type high-energy ultrasonic method was used to crush the sugar beet pulp. The ultrasonic power is 190 W/cm 2 , the treatment time is 12 min, the ultrasonic duration is 2 s, and the interval is 2 s. In the process, mechanical stirring at 400 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath. The temperature of the suspension should not exceed 45°C during treatment. The obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt%~15wt% and then spray-dried to obtain a full-component emulsified thickening agent for sugar beet pulp.
使用：产品粉末分散于水中形成浓度为2.5wt%的悬液，采用高速剪切均质的方法对悬液进行均质，转速为19000~20000 rpm，均质时间为5 min，而后采用机械搅拌的方式在450~500 rpm转速下搅拌8 h。所得悬液可稀释后或直接用于乳化增稠。Usage: The product powder is dispersed in water to form a suspension with a concentration of 2.5wt%. The suspension is homogenized using high-speed shear homogenization method with a rotation speed of 19000~20000. rpm, the homogenization time is 5 minutes, and then mechanical stirring is used at 450~500 Stir at rpm speed for 8 h. The resulting suspension can be diluted or directly used for emulsification and thickening.
本实施例所制备的甜菜粕全组分乳化剂可溶性固形物比例为43.2wt%，其中可溶性果胶组分含量为28.6wt%，可溶性果胶的分子量为459 kDa，如表1所示。不溶性组分解离为直径为50~200 nm，长度为3~50μm不等的纳米纤维丝。所得产品在0.5wt%的浓度下外观为均匀不分层的纤维胶体絮状物，胶体稳定性良好，而原始甜菜粕分层明显且几乎不发生溶胀，呈块状结构；0.5wt%的本实施例产品的表观粘度1.225 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.021 Pa·s。0.5wt%浓度下的本实施例产品可制备20wt%的玉米油乳液，其乳液粒径 d 4,3为6.13 μm，乳液在室温下存放60天乳液粒径 d 4,3为6.18 μm，乳液没有发生明显乳析分层现象，乳化稳定性良好。作为对照的甜菜果胶在0.5wt%浓度下单独制备20wt%的玉米油液，其乳液粒径 d 4,3为1.21 μm，乳液在室温下存放60天乳液粒径 d 4,3为25.5 μm，乳液出现明显乳析分层，乳化稳定性较差。 The soluble solids ratio of the full-component emulsifier of sugar beet meal prepared in this example is 43.2wt%, of which the soluble pectin component content is 28.6wt%, and the molecular weight of the soluble pectin is 459 kDa, as shown in Table 1. The insoluble components dissociate into nanofiber filaments with diameters of 50 to 200 nm and lengths of 3 to 50 μm. At a concentration of 0.5wt%, the obtained product appears as a uniform non-stratified fibrous colloid floc with good colloid stability, while the original sugar beet pulp is obviously stratified and almost does not swell, showing a massive structure; 0.5wt% The apparent viscosity of the product in this example is 1.225 Pa·s, while the apparent viscosity of the original sugar beet pulp and the control sugar beet pectin at the same concentration are 0.008 Pa·s and 0.021 Pa·s. The product of this example at a concentration of 0.5wt% can prepare a 20wt% corn oil emulsion. The emulsion particle size d 4,3 is 6.13 μm. When the emulsion is stored at room temperature for 60 days, the emulsion particle size d 4,3 is 6.18 μm. No obvious emulsion stratification occurred, and the emulsification stability was good. As a control, 20wt% corn oil liquid was prepared separately from sugar beet pectin at a concentration of 0.5wt%. The emulsion particle size d 4,3 was 1.21 μm. The emulsion particle size d 4,3 was 25.5 μm after being stored at room temperature for 60 days. , the emulsion showed obvious emulsion stratification, and the emulsion stability was poor.
对比例1：Comparative example 1:
制备：除杂、烘干、粉碎同实施例1。所得甜菜粕粉末(过100目筛)加水分散形成浓度约为5wt%，总体积为5 L的甜菜浆，而后采用探头式高能超声法对甜菜粕进行破碎处理。超声功率127 W/cm 2，处理时间30 min，超声持续时间2 s，间隔2 s，该过程中采用600 rpm转速机械搅拌向体系中混入少量气泡使体系被超声均匀处理且以冰水浴进行冷却使悬浊液在处理过程中温度不超过45 ℃。所得粘稠悬浊液可采用膜浓缩或减压浓缩至浓度为13wt%~15wt%后进行喷雾干燥得对比例2乳化增稠剂。 Preparation: impurity removal, drying, and crushing are the same as in Example 1. The obtained sugar beet pulp powder (passed through a 100-mesh sieve) is dispersed with water to form a sugar beet pulp with a concentration of approximately 5 wt% and a total volume of 5 L. The sugar beet pulp is then crushed using a probe-type high-energy ultrasonic method. The ultrasonic power is 127 W/cm 2 , the treatment time is 30 min, the ultrasonic duration is 2 s, and the interval is 2 s. In the process, mechanical stirring at 600 rpm is used to mix a small amount of bubbles into the system so that the system is uniformly treated by ultrasonic and cooled with an ice water bath. The temperature of the suspension should not exceed 45°C during treatment. The obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt%~15wt% and then spray-dried to obtain the emulsified thickener of Comparative Example 2.
使用：同实施例1。Usage: Same as Example 1.
本对比例所制备的乳化增稠剂可溶性固形物比例为18.6wt%，其中可溶性果胶组分含量为10.2wt%，可溶性果胶的分子量为516 kDa，如表1所示。其光学显微镜照显示其为直径达十几至几十微米的、表面具有规则边缘的块状颗粒（如图8所示）。所得产品在0.5wt%的浓度下外观为沉淀物，胶体稳定性差，与分层明显的原始甜菜粕相似（图9，图9中a为对比例1的产品悬浮液外观图，图9中b为原始甜菜粕粉末悬浮液外观图）；0.5wt%的本对比例产品的表观粘度为0.011 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.022 Pa·s，本对比例产品增稠性差。0.5wt%浓度下的本对比例产品可以制备出的20 wt%的玉米油乳液，但其在均质后发生快速的分层，有部分油明显析出，乳液粒径 d 4,3为78.6 μm，乳化活性差。图6是本对比例制备乳液的显微镜图，大量颗粒没有全部吸附到油滴界面上，仅有少量圆球状乳液滴在视野中，其乳液形成机理如图7中b所示。块状颗粒不具有柔韧性，直径大导致其难以吸附到油滴表面，且无法与共同吸附到界面上的水溶性果胶形成网状结构，其界面膜脆弱且容易暴露油滴，导致乳液性质差。乳液在室温下存放仅7天后乳液析油加剧且乳液粒径无法测定，乳化稳定性差。 The soluble solids ratio of the emulsified thickener prepared in this comparative example is 18.6wt%, of which the soluble pectin component is 10.2wt%, and the molecular weight of the soluble pectin is 516 kDa, as shown in Table 1. Its optical microscope photo shows that it is a massive particle with a diameter of more than ten to tens of microns and a regular edge on the surface (as shown in Figure 8). The appearance of the obtained product is a sediment at a concentration of 0.5wt%, with poor colloidal stability, similar to the original sugar beet meal with obvious stratification (Figure 9, a in Figure 9 is the appearance of the product suspension of Comparative Example 1, Figure 9 b is the appearance of the original sugar beet meal powder suspension); the apparent viscosity of 0.5wt% of this comparative product is 0.011 Pa·s, while the apparent viscosity of the original sugar beet meal and control sugar beet pectin at the same concentration is 0.008 Pa·s and 0.022 Pa·s, the product of this comparative example has poor thickening properties. The product of this comparative example at a concentration of 0.5wt% can prepare a 20 wt% corn oil emulsion, but it rapidly stratifies after homogenization, and some oil is obviously separated out. The emulsion particle size d 4,3 is 78.6 μm. , poor emulsifying activity. Figure 6 is a microscope picture of the emulsion prepared in this comparative example. A large number of particles are not all adsorbed to the oil droplet interface, and only a small amount of spherical emulsion droplets are in the field of view. The emulsion formation mechanism is shown in b in Figure 7. The massive particles are not flexible, and their large diameter makes it difficult to adsorb to the surface of the oil droplets, and they cannot form a network structure with the water-soluble pectin co-adsorbed to the interface. The interface film is fragile and the oil droplets are easily exposed, resulting in emulsion properties. Difference. After the emulsion was stored at room temperature for only 7 days, oil separation from the emulsion intensified and the particle size of the emulsion could not be determined, resulting in poor emulsion stability.
对比例2Comparative example 2
制备：除杂、烘干、粉碎同实施例1。取甜菜粕粉末(过100目筛)分散于水形成浓度约为20wt%的甜菜粕悬液，置于高压反应釜中以110~120 ℃处理4 h。所得悬浊液稀释浓度质13wt%~15wt%后进行喷雾干燥得对照例1乳化增稠剂。Preparation: impurity removal, drying, and crushing are the same as in Example 1. Take the sugar beet pulp powder (passed through a 100 mesh sieve) and disperse it in water to form a sugar beet pulp suspension with a concentration of about 20wt%. Place it in a high-pressure reactor at 110~120 ℃ treatment for 4 h. The obtained suspension was diluted to a concentration of 13wt% to 15wt% and then spray-dried to obtain the emulsified thickener of Comparative Example 1.
使用：同实施例1。Usage: Same as Example 1.
本对比例所制备的乳化增稠剂可溶性固形物比例为23.1wt%，其中可溶性果胶组分含量为14.4wt%，可溶性果胶的分子量为528 kDa，如表1所示。不溶性组分为表面规则的块状颗粒。所得产品在0.5wt%的浓度下外观为沉淀物，胶体稳定性差，与分层明显的原始甜菜粕相似；0.5wt%的本对比例产品的表观粘度为0.009 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.022 Pa·s，本对比例产品不具有增稠性。0.5wt%浓度下的本对比例产品不能制备出稳定的20 wt%的玉米油乳液，其在均质后发生快速分层并大量析出油，乳液粒径无法测定，不具有乳化能力。The soluble solids ratio of the emulsified thickener prepared in this comparative example is 23.1wt%, of which the soluble pectin component content is 14.4wt%, and the molecular weight of the soluble pectin is 528 kDa, as shown in Table 1. The insoluble components are massive particles with regular surfaces. The obtained product appears as a sediment at a concentration of 0.5wt%, with poor colloidal stability, similar to the original sugar beet meal with obvious stratification; the apparent viscosity of the comparative product at 0.5wt% is 0.009 Pa·s, while the original sweetened The apparent viscosity of rapeseed meal and control sugar beet pectin at the same concentration are 0.008 Pa·s and 0.022 Pa·s. The product of this comparative example has no thickening property. The product of this comparative example at a concentration of 0.5wt% cannot produce stable 20 The wt% corn oil emulsion quickly stratifies and precipitates a large amount of oil after homogenization. The particle size of the emulsion cannot be measured and it has no emulsifying ability.
对比例3Comparative example 3
制备：除杂、烘干、粉碎同实施例1。取甜菜粕粉末分散于水形成浓度约为20wt%的甜菜粕悬液，置于高压反应釜中以110~120 ℃处理4 h。所得甜菜粕粉末加水分散形成浓度约为5wt%，总体积为5 L的甜菜浆，而后采用槽式超声法清洗仪对甜菜粕进行低能超声处理处理。超声功率为0.88 W/cm 2，超声连续处理时间30 min，该过程中采用600 rpm转速机械搅拌向体系中混入少量气泡使体系被超声均匀处理。所得粘稠悬浊液可采用膜浓缩或减压浓缩至浓度为13wt%~15wt%后进行喷雾干燥得得对照例3乳化增稠剂。 Preparation: impurity removal, drying, and crushing are the same as in Example 1. Disperse the sugar beet pulp powder in water to form a sugar beet pulp suspension with a concentration of approximately 20wt%, and place it in a high-pressure reaction kettle for treatment at 110~120°C for 4 hours. The obtained sugar beet pulp powder was dispersed with water to form a sugar beet pulp with a concentration of about 5wt% and a total volume of 5 L. The sugar beet pulp was then treated with low-energy ultrasonic treatment using a tank-type ultrasonic cleaner. The ultrasonic power was 0.88 W/cm 2 and the continuous ultrasonic treatment time was 30 min. During the process, mechanical stirring at 600 rpm was used to mix a small amount of bubbles into the system to make the system uniformly treated by ultrasonic. The obtained viscous suspension can be concentrated by membrane or reduced pressure to a concentration of 13wt%~15wt% and then spray-dried to obtain the emulsified thickener of Comparative Example 3.
使用：同实施例1Usage: Same as Example 1
本对照例所制备的乳化增稠剂可溶性固形物比例为26.7 wt%，其中可溶性果胶组分含量为16.2 wt%，可溶性果胶的分子量为532 kDa，如表1所示。不溶性组分为表面规则的块状颗粒。所得产品在0.5wt%的浓度下外观为沉淀物，胶体稳定性差，与分层明显的原始甜菜粕相似；0.5wt%产品的表观粘度为0.013 Pa·s，而原始甜菜粕和对照甜菜果胶在相同浓度下表观粘度为0.008 Pa·s和0.022 Pa·s，本对比例产品增稠性差。0.5%浓度下的本对比例产品不能制备出稳定的20wt%的玉米油乳液，其在均质后发生快速分层并大量析出油，乳液粒径无法测定，不具有乳化能力。The soluble solids ratio of the emulsified thickener prepared in this comparative example is 26.7 wt%, of which the soluble pectin component content is 16.2 wt%, the molecular weight of soluble pectin is 532 kDa, as shown in Table 1. The insoluble components are massive particles with regular surfaces. The obtained product looks like a precipitate at a concentration of 0.5wt%, with poor colloidal stability, similar to the original beet meal with obvious stratification; the apparent viscosity of the 0.5wt% product is 0.013 Pa·s, while the original beet meal and the control The apparent viscosity of sugar beet pectin at the same concentration is 0.008 Pa·s and 0.022 Pa·s, and the product of this comparative example has poor thickening properties. The product of this comparative example at a concentration of 0.5% cannot prepare a stable 20wt% corn oil emulsion. After homogenization, it rapidly stratifies and precipitates a large amount of oil. The particle size of the emulsion cannot be measured and it does not have emulsifying ability.
表1Table 1
相比于一般超声处理，如中国发明专利（CN20130381569.2）提及的静电场（8~32kV）与较弱超声（0.35~0.88W/cm 2）联合处理，其可以促进果胶的溶出用于提取甜菜果胶，但是弱超声作用并不能有效破碎甜菜粕使其解离为丝状纳米纤维，所剩余的甜菜粕颗粒仍为大颗粒，胶体稳定性差且乳化性差。 Compared with general ultrasonic treatment, the combined treatment of electrostatic field (8~32kV) and weaker ultrasound (0.35~0.88W/cm 2 ) mentioned in the Chinese invention patent (CN20130381569.2) can promote the dissolution of pectin. It is used to extract beet pectin, but the weak ultrasonic effect cannot effectively break up the beet pulp and dissociate it into filamentous nanofibers. The remaining sugar beet pulp particles are still large particles with poor colloidal stability and poor emulsification.
本发明制备出的甜菜粕全组分乳化增稠剂既含有分子量大且分子结构完整的可溶性果胶分子，其具有良好的乳化活性；也含有长度为数十微米，直径为纳米级的纳米纤维丝，具有长径比更大，弯曲柔韧性好的特点，其能在在球状油滴表面可以自由弯曲紧密贴合。而没有解离为纳米丝的颗粒状的甜菜粕由于颗粒直径约有数微米，其刚性颗粒吸附贴合在油滴表面的面积远小于具有弯曲柔韧性的纳米丝，导致其不仅因吸附能过大而难以吸附到油滴表面，且用于稳定相同面积的油滴所需要的颗粒量远远大于丝状的甜菜粕，虽可与可溶性果胶共同吸附在油滴上，其乳液的粒径更大，更容易发生分层失稳的现象。而细丝状纳米纤维与果胶大分子共同吸附在乳液表面时，纳米级的直径使得细丝纤维吸附能降低而快速紧密贴合在油滴表面，从而形成相互交错的网状界面膜结构，纤维丝之间的间隙被大分子果胶组分所覆盖，两者协同形成紧密的网状界面膜，阻止因油滴暴露而诱发的油滴失稳，提高乳液稳定性。The whole-component emulsifying thickener of beet pulp prepared by the invention not only contains soluble pectin molecules with large molecular weight and complete molecular structure, which have good emulsifying activity; it also contains nanometer-sized molecules with a length of tens of micrometers and a diameter of nanometers. Fiber filaments have the characteristics of larger aspect ratio and good bending flexibility. They can freely bend and fit tightly on the surface of spherical oil droplets. The granular sugar beet pulp that has not been dissociated into nanowires has a particle diameter of about several microns, and the area of its rigid particles adsorbed on the surface of the oil droplets is much smaller than that of nanowires with bending flexibility. As a result, not only does the adsorption energy exceed It is large and difficult to adsorb to the surface of oil droplets, and the amount of particles required to stabilize oil droplets of the same area is much larger than that of filamentous sugar beet pulp. Although it can be adsorbed on oil droplets together with soluble pectin, the particle size of its emulsion The larger the diameter, the more prone to delamination instability. When filamentous nanofibers and pectin macromolecules are co-adsorbed on the emulsion surface, the nanometer-scale diameter reduces the adsorption energy of the filamentary fibers and quickly and closely adheres to the surface of the oil droplets, thereby forming an intertwined network interface film structure. The gaps between the fiber filaments are covered by macromolecular pectin components, and the two work together to form a tight network interface film, which prevents the instability of oil droplets caused by exposure of oil droplets and improves the stability of the emulsion.
相比之下，中国发明专利申请CN202110463660.3公开了一种采用传统热酸法分离果胶，而后采用胶体磨及酶法来破碎柑橘膳食纤维，制备出具有皮克林乳化性的纳米粒径柑橘纤维。中国发明专利申请CN201811377985.4公开了一种水热-超声破碎法制备纳米级不溶性大豆多糖的方法，采用pH 3.5的弱酸对大豆粕进行可溶性多糖的脱除，仅获得大豆不溶性多糖的纳米颗粒。后两者均对不溶性纤维进行精制分离，只关注了不溶性纤维的乳化性而忽略了其与可溶性组可能存在的协同乳化增稠作用，且生产过程需要用到强酸强碱等化学试剂，增加成本且环境不友好。In contrast, Chinese invention patent application CN202110463660.3 discloses a method that uses a traditional hot acid method to separate pectin, and then uses a colloid mill and enzymatic method to crush citrus dietary fiber to prepare nanoparticles with Pickering emulsification properties. Citrus fiber. Chinese invention patent application CN201811377985.4 discloses a method for preparing nanoscale insoluble soybean polysaccharide by hydrothermal-ultrasonic crushing method, using pH The weak acid of 3.5 was used to remove soluble polysaccharides from soybean meal, and only nanoparticles of insoluble soybean polysaccharides were obtained. The latter two both refine and separate insoluble fiber, focusing only on the emulsifying properties of insoluble fiber and ignoring the possible synergistic emulsification and thickening effects of it and the soluble group. Moreover, the production process requires the use of chemical reagents such as strong acids and alkalis, which increases costs. And the environment is not friendly.
综合而言，本发明采用无化学试剂添加的水热物理法从甜菜粕中同时获取结构完整的大分子甜菜果胶及解离彻底的纳米纤维丝，两者协同可实现良好的乳化增稠性In summary, the present invention uses a hydrothermal physical method without the addition of chemical reagents to simultaneously obtain structurally intact macromolecular sugar beet pectin and completely dissociated nanofibers from sugar beet pulp. The synergy of the two can achieve good emulsification and thickening. sex

Claims (10)

  1. 一种甜菜粕全组分乳化增稠剂的制备方法，其特征在于包括如下步骤：A method for preparing a full-component emulsifying thickener of beet pulp, which is characterized by comprising the following steps:
    1）清洗粉碎预处理； 1) Cleaning and crushing pretreatment;
    2）取清洗粉碎预处理后的甜菜粕粉末分散于水中，置于高压反应釜中控制温度为110~140℃水热处理0.5~4 h；2) Disperse the cleaned, crushed and pre-treated sugar beet meal powder in water, place it in a high-pressure reactor and control the temperature to 110~140°C for hydrothermal treatment for 0.5~4 hours;
    3）向步骤2）获得的水热处理甜菜粕分散液中加水稀释后搅拌的同时进行高能超声破碎处理；3) Add water to dilute the hydrothermally treated beet pulp dispersion obtained in step 2) and perform high-energy ultrasonic crushing while stirring;
    4）对步骤3）获得的超声破碎甜菜粕分散液进行浓缩后干燥，获得甜菜粕全组分乳化增稠剂。4) Concentrate and then dry the ultrasonic crushed beet pulp dispersion obtained in step 3) to obtain a full-component emulsifying thickener of sugar beet pulp.
  2. 根据权利要求1所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：所述的清洗粉碎预处理是将甜菜压粕在水中浸泡直至甜菜丝吸水发胀分散，去除其中包括泥土木屑在内的杂质及焦黑甜菜丝，再将甜菜粕从水中捞出除去部分水分后烘干，将干燥甜菜粕粉碎过筛后置于阴凉处备用。The preparation method of beet pulp full-component emulsifying thickener according to claim 1, characterized in that: the cleaning and crushing pretreatment is to soak the sugar beet pulp in water until the beet shreds absorb water, swell and disperse, and remove the Impurities including soil and sawdust and burnt beet shreds are removed from the water, and then the beet pulp is removed from the water to remove part of the water and then dried. The dried beet pulp is crushed and screened and placed in a cool place for later use.
  3. 根据权利要求2所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：所述的除去部分水是采用螺旋挤压机进行；所述的烘干是在烘箱进行；控制烘干的温度为45~65 ℃，时间为10~24 h，甜菜粕干燥后的水分含量为6wt%~9wt%。The preparation method of beet pulp full-component emulsifying thickener according to claim 2, characterized in that: the removal of part of the water is carried out by using a screw extruder; the drying is carried out in an oven; control The drying temperature is 45~65°C and the drying time is 10~24 h. The moisture content of the dried sugar beet pulp is 6wt%~9wt%.
  4. 根据权利要求2所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：干燥甜菜粕粉碎过筛的筛网目数为100~400目。The preparation method of the whole-component emulsifying thickener of beet pulp according to claim 2, characterized in that: the mesh size of the crushed and sieved dried sugar beet pulp is 100 to 400 meshes.
  5. 根据权利要求1所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：所述的清洗粉碎预处理后的甜菜粕粉末分散于水中所形成的甜菜粕悬液浓度为2wt%~20wt%。The preparation method of the whole-component emulsifying thickener of beet meal according to claim 1, characterized in that: the concentration of the beet meal suspension formed by dispersing the washed, crushed and pretreated beet meal powder in water It is 2wt%~20wt%.
  6. 根据权利要求1所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：所述的水热处理温度为120~130℃，时间为1-1.5 h。The preparation method of beet pulp full-component emulsifying thickener according to claim 1, characterized in that: the hydrothermal treatment temperature is 120~130°C and the time is 1-1.5 h.
  7. 根据权利要求1所述的甜菜粕全组分乳化增稠剂的制备和使用方法，其特征在于：加水稀释后的水热处理甜菜粕分散液的浓度为0.5wt%~5wt%；所述的高能超声破碎处理的功率密度为127~255 W/cm 2，时间为5~25 min；所采用的高能超声破碎处理模式为持续2 s，间隔2 s，处理过程中水热处理甜菜粕分散液采用200～600rpm转速机械搅拌，搅拌在敞口容器中进行，且以-4~4℃循环冰水浴进行冷却使体系温度不高于45℃。 The preparation and use method of the beet pulp full-component emulsifying thickener according to claim 1, characterized in that: the concentration of the hydrothermally treated sugar beet pulp dispersion diluted with water is 0.5wt%~5wt%; The power density of the high-energy ultrasonic crushing treatment is 127~255 W/cm 2 and the time is 5~25 min; the high-energy ultrasonic crushing treatment mode used is 2 s continuous and 2 s apart. During the treatment process, the hydrothermal treatment of beet pulp is dispersed The liquid is mechanically stirred at a speed of 200 to 600 rpm, and the stirring is carried out in an open container, and is cooled in a -4 to 4°C circulating ice water bath to keep the system temperature no higher than 45°C.
  8. 根据权利要求1所述的甜菜粕全组分乳化增稠剂的制备方法，其特征在于：所述的浓缩的方式采用减压浓缩或超滤膜过滤浓缩；当浓缩至13wt%~15wt%时采用喷雾干燥的方法进行干燥。The preparation method of beet pulp full-component emulsifying thickener according to claim 1, characterized in that: the concentration method adopts reduced pressure concentration or ultrafiltration membrane filtration concentration; when concentrated to 13wt%~15wt% The spray drying method is used for drying.
  9. 一种甜菜粕全组分乳化增稠剂，其特征在于，其由权利要求1-8任一项所述的制备方法制得，所得甜菜粕全组分乳化增稠剂的可溶性组分含量为39.5wt%~45.1wt%，可溶性果胶含量为24.3wt%~29.7wt%，可溶果胶的分子量为392~561kDa，并含有香味，纤维是直径为50~200 nm，长度为3~50 μm的条状纳米纤维丝。A kind of beet meal full-component emulsifying thickener, characterized in that it is prepared by the preparation method described in any one of claims 1 to 8, and the soluble component of the obtained beet meal full-component emulsifying thickener is The content is 39.5wt%~45.1wt%, the soluble pectin content is 24.3wt%~29.7wt%, the molecular weight of soluble pectin is 392~561kDa, and contains fragrance. The fiber has a diameter of 50~200 nm and a length of 3 ~50 μm strip nanofibers.
  10. 权利要求9所述的甜菜粕全组分乳化增稠剂对含脂酱料、奶油或酸奶乳化增稠的应用；其特征在于，甜菜粕全组分乳化增稠剂在用于乳化增稠前进行充分的分散和水化。The application of the whole-component emulsifying thickener of beet pulp according to claim 9 for emulsifying and thickening fat-containing sauces, cream or yogurt; It is characterized in that the whole-component emulsifying thickening agent of beet pulp is used for emulsifying and thickening. Fully disperse and hydrate before thickening.
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