CN112741299A - Food-grade temperature-sensitive pickering emulsion and preparation method thereof - Google Patents
Food-grade temperature-sensitive pickering emulsion and preparation method thereof Download PDFInfo
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- CN112741299A CN112741299A CN202011567257.7A CN202011567257A CN112741299A CN 112741299 A CN112741299 A CN 112741299A CN 202011567257 A CN202011567257 A CN 202011567257A CN 112741299 A CN112741299 A CN 112741299A
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- 238000001484 Pickering emulsion method Methods 0.000 title description 2
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- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 claims description 2
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- 229940100486 rice starch Drugs 0.000 claims description 2
- 229940032147 starch Drugs 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- PHXATPHONSXBIL-UHFFFAOYSA-N xi-gamma-Undecalactone Chemical compound CCCCCCCC1CCC(=O)O1 PHXATPHONSXBIL-UHFFFAOYSA-N 0.000 claims description 2
- WTEVQBCEXWBHNA-YFHOEESVSA-N neral Chemical compound CC(C)=CCC\C(C)=C/C=O WTEVQBCEXWBHNA-YFHOEESVSA-N 0.000 claims 1
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Images
Classifications
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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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/72—Encapsulation
-
- 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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/80—Emulsions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
-
- 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
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- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a food-grade temperature-sensitive Pickering emulsion and a construction method thereof, belonging to the technical field of emulsion preparation. The temperature-sensitive Pickering emulsion comprises edible wax modified starch nanocrystal, flavor components and water. The preparation method comprises the following steps: mixing the edible wax modified starch nanocrystal, the flavor components and water to obtain a mixed solution, then dispersing at a high speed, and dispersing the mixed solution by combining high-pressure homogenization or high-pressure microjet to prepare the temperature-sensitive Pickering emulsion. The pickering emulsion prepared by the invention can be used as a safe and effective flavor component sustained and controlled release system.
Description
Technical Field
The invention belongs to the technical field of emulsion preparation, and particularly relates to a food-grade temperature-sensitive pickering emulsion and a preparation method thereof.
Background
The application of the microcapsule technology in stabilizing the food flavors and fragrances overcomes the defects of easy volatilization and instability of the food flavors and fragrances to a great extent. At present, microencapsulated essence and flavor at home and abroad occupies more than half of the total consumption of the essence, the encapsulation technology has great improvement on the characteristics of the essence such as protection, water dispersibility and the like, but the release of the essence after the encapsulation is ignored by people. Because the essence is released mainly by the rupture of the vesicle, and most of the capsule walls adopt water-soluble materials, the fragrance of the microencapsulated product is easy to release suddenly due to dissolution when in use, and the lasting and controlled release characteristics of the fragrance cannot be achieved. Therefore, the construction of corresponding temperature-sensitive essence encapsulated products aiming at the requirements of food systems is the key point of the steady-state technology research of the essence at present.
For temperature-sensitive carriers, various emulsification technologies mainly based on temperature-sensitive high polymer materials such as poly-N-isopropylacrylamide are currently researched at home and abroad, and the temperature-sensitive carriers are widely researched in the aspects of drug delivery, immobilized enzymes, immunoassay and the like. However, the temperature sensitivity range of the system given by the material is limited, and the requirements of different food systems on the release of the material cannot be met. Therefore, how to develop a natural and broad-spectrum temperature-sensitive material and construct a related carrier by taking the material as a substrate is a key problem to be solved in the field. The patent adopts edible starch as a raw material, firstly prepares the starch nanocrystal, reduces the size of the granule and is more beneficial to subsequent modification. And secondly, combining the high hydrophobicity of the wax, carrying out hydrophobic modification on the starch nanocrystal and improving the emulsifying activity of the starch nanocrystal. And finally, the particles are endowed with a certain temperature sensitive characteristic by combining different melting temperature characteristics of different types of wax, so that a stable system of the particles also has a relevant temperature sensitive characteristic.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a food-grade temperature-sensitive pickering emulsion and a preparation method thereof. The pickering emulsion can be used as a safe and effective flavor component sustained and controlled release system.
The technical scheme of the invention is as follows:
the food-grade temperature-sensitive pickering emulsion comprises the following components in percentage by mass: 0.1-10% of edible wax modified starch nanocrystal, 10-60% of flavor components and the balance of water.
The edible wax modified starch nanocrystal comprises the following steps: dissolving edible wax, stirring, adding the starch nanocrystal, stirring, mixing, reacting, adding deionized water with the same temperature as a reaction system, flushing the starch nanocrystal into an ice-water bath of the system, collecting a sample, centrifuging, drying a precipitate in vacuum, grinding and crushing to finally obtain the starch nanocrystal with the hydrophobically modified surface, namely the wax modified starch nanocrystal.
The starch nanocrystal is prepared by hydrolyzing raw starch granules with concentrated sulfuric acid, wherein the raw starch granules are one or more of waxy corn starch, common corn starch, cassava starch, potato starch, rice starch or wheat starch.
The edible wax is one or more of paraffin, beeswax, carnauba wax, ceresin, Chinese wax, rice bran wax, sunflower wax or lacquer wax.
The paraffin wax is at least one of 52, 54, 56, 58, 60, 62, 64 or 66 in grade.
The flavor components are one or more of beta-ionone, beta-sweet orange aldehyde, beta-pinene, citral, eugenol or peach aldehyde.
The preparation method of the food-grade temperature-sensitive pickering emulsion comprises the following steps: mixing the edible wax modified starch nanocrystal, the flavor components and water to obtain a mixed solution, then dispersing at a high speed, and dispersing the mixed solution by combining high-pressure homogenization or high-pressure microjet to prepare the temperature-sensitive Pickering emulsion.
The high-speed dispersion rotating speed is 10000-22000 rpm, and the dispersion time is 2-5 min.
The pressure of the high-pressure homogenization is 30-150 MPa, and the homogenization times are 3-10 times.
The pressure of the high-pressure micro-jet is 30-100 MPa, and the number of times of micro-jet is 2-5.
The beneficial technical effects of the invention are as follows:
the invention creatively combines the high hydrophobicity and the high-temperature melting characteristic of the edible wax, carries out surface physical hydrophobic modification on the natural granular emulsifier-starch nanocrystal, and combines the Pickering emulsion as a matrix to entrap flavor components. On the basis of endowing starch nanocrystals with certain hydrophobic characteristics, the starch nanocrystals have temperature-sensitive characteristics. According to the selection of edible waxes with different melting points, the hydrophobic wax layer on the surface of the particle can be melted at the corresponding melting point temperature, so that the stability of the pickering emulsion is changed, and the flavor components are released. The technology belongs to physical modification, the modification process is simple and controllable, food-grade raw materials are selected, and the technology has a wide application prospect in the field of food additives.
Meanwhile, in the modification process, the invention solves a key problem in the field, namely how to separate the modified starch nanocrystals from the redundant waxes.
The method creatively selects the Pickering emulsion as a temperature sensitive carrier matrix, and takes the starch nanocrystals modified by the edible wax as a particle emulsifier, and the physical modification scheme is safe and controllable, enhances the hydrophobicity of the surface of the starch nanocrystals, improves the emulsifying activity of the starch nanocrystals, and further endows the particles with temperature sensitivity. When the emulsion is heated to a temperature higher than the melting point of the edible wax, the original stability of the pickering emulsion is changed due to the melting of the wax, and further the flavor components in the carrier are released. The pickering emulsion can be used as a safe and effective flavor component sustained and controlled release system, endows the system with a specific release temperature through selection of edible waxes with different melting points, and has a good application prospect in the aspect of food additives.
Drawings
FIG. 1 is a diagram of a modification reaction apparatus of starch nanocrystals in example 2;
FIG. 2 is a three-phase contact angle measurement chart of the carnauba wax/waxy corn starch nanocrystal composite particle, with the reaction times of 5min, 30min, 60min and 120min, respectively;
FIG. 3 is a photograph of Pickering emulsion prepared from carnauba wax/waxy corn starch nanocrystalline composite particles, with modification times of 5min, 30min and 60min, respectively;
FIG. 4 is a Pickering emulsion microscope photograph of potato starch nanocrystal/paraffin (52) composite particles, with reaction times of (A)5min, (B)30min and (C)60 min;
FIG. 5 is the flavor release profile of the beta-ionone pickering emulsion of example 5 at different temperatures;
figure 6 is a graph of the flavor release profiles of the citral pickering emulsion of example 6 at different temperatures.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit and scope of the present invention, and it is therefore not intended that the present invention be limited to the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
30g of waxy corn starch was accurately weighed, placed in a 250mL round bottom flask, and 150mL (3.16 mol/L) of H was added2SO4The solution is hydrolyzed and stirred at 400r/min, the reaction temperature is 40 ℃, and the reaction time is 5 days. After the reaction is finished, washing and centrifuging the obtained product for many times until the pH value of the supernatant is about 6.8, and freeze-drying the obtained waxy corn starch crystal solution to obtain powder which is stored at room temperature for later use.
Example 2
As shown in FIG. 1, the reaction apparatus was first closed, 30mL of deionized water was measured and added to a three-necked flask, 10g of carnauba wax was added, and circulating water at 85. + -. 1 ℃ was introduced to start stirring. Stirring for a period of time until the solid carnauba wax is completely dissolved, stopping stirring, separating the upper oil phase from the lower oil phase, and opening a valve to remove the lower water phase. Accurately weighing 5g of waxy corn starch nanocrystalline in example 1, adding the waxy corn starch nanocrystalline into a three-neck flask, stirring at the rotation speed of 80r/min, reducing the rotation speed after stirring for 5min, 30min, 60min and 120min, adding 30mL of water with the temperature of 85 +/-1 ℃ into the three-neck flask, stopping stirring after continuously stirring for 5s, opening a valve, and quickly separating the lower-layer starch water dispersion liquid into a beaker placed in an ice-water bath. Centrifuging the prepared starch nanocrystal aqueous dispersion for 10min at the rotating speed of 3500r/min, removing supernatant, and freeze-drying the obtained solid for later use.
And (3) taking waxy corn starch nanocrystals with modification time of 5min, 30min, 60min and 120min respectively, and preparing into a wafer with thickness of 1-2 mm by using a tablet press, wherein the pressure is 15Mpa and the time is 5 min. The contact angle was measured using an optical contact angle measuring instrument model OCA40 equipped with a CDD camera, and the number of parallel measurements was not less than 5. As shown in FIG. 2, it can be seen from the trend of the change in contact angle that the value of the contact angle increases with the increase of the modification time, but the bound contact angle decreases when the reaction time is 120 min. Taking waxy corn starch nanocrystals with modification time of 5min, 30min and 60min respectively, preparing 25g of 1% solution with deionized water, ultrasonically dispersing for 0.5h, and standing for 24 h. Selecting beta-ionone as a representative flavor component, taking 10g of beta-ionone, uniformly stirring the beta-ionone and the modified waxy corn starch nanocrystals, and preparing the Pickering emulsion by high-speed dispersion and high-pressure homogenization.
Example 3
The preparation method comprises the following steps of taking 5g of potato starch nanocrystals, carrying out physical hydrophobic modification on the potato starch nanocrystals and paraffin (No. 52) by adopting the operation in the example 2, and selecting 60min as modification time to obtain the paraffin-modified potato starch nanocrystals.
Preparing 25g of solution with the concentration of 1% by using deionized water, ultrasonically dispersing for 0.5h, and standing for 24 h. Selecting citral as a representative flavor component, taking 10g of limonene, uniformly stirring with the modified waxy corn starch nanocrystals, and preparing pickering emulsion by adopting high-speed dispersion and high-pressure homogenization.
Example 4
Taking 0.25g of wheat starch nanocrystal, carrying out physical hydrophobic modification on the wheat starch nanocrystal and paraffin (No. 60) by adopting the operation in the embodiment 2, and selecting 60min as modification time to obtain the paraffin modified wheat starch nanocrystal.
Taking the prepared paraffin modified wheat starch nanocrystal, preparing 25g of 2% solution by using deionized water, ultrasonically dispersing for 0.5h, and standing for 24 h. Selecting beta-pinene as a representative flavor component, taking 20g of beta-pinene, uniformly stirring the beta-pinene and the modified wheat starch nanocrystals, and preparing the Pickering emulsion by adopting high-speed dispersion and high-pressure homogenization.
Example 5
The Pickering emulsion prepared from the waxy corn starch nanocrystal/carnauba wax composite particles modified for 60min in example 2 was taken, placed in a gas headspace bottle, and the release of beta-ionone at different temperatures (50 ℃, 60 ℃, 80 ℃ and 90 ℃) was determined by GC-MS headspace gas chromatography.
A chromatographic column: TG-WAXMS (30 m.times.0.25 mm.times.0.25 μm), Thermo corporation, USA; chromatographic analysis conditions: the injector temperature was 250 ℃; the temperature of the transmission line is 250 ℃ and the temperature of the ion source is 280 ℃; flow rate: 1.2 mL/min; EI 70 ev; temperature programming conditions: from 100 ℃ to 230 ℃ at a rate of 10 ℃/min.
The release profile of beta-ionone is shown in fig. 5, when the pickering emulsion is heated to 90 ℃, the release amount of beta-ionone reaches the maximum, while the release amount at 80 ℃ and 60 ℃ is significantly reduced, and when the temperature is 50 ℃, the release of beta-ionone is almost not released.
Example 6
The Pickering emulsion prepared in example 4 was taken, placed in a gas headspace bottle and the release of citral at different temperatures (25 ℃, 35 ℃, 42 ℃ and 50 ℃) was determined by GC-MS headspace gas chromatography. As a result, as shown in FIG. 6, the amount of released limonene reached a maximum when the Pickering emulsion was heated to 42 ℃ and 50 ℃ and almost no release occurred at 25 ℃ and 35 ℃.
The experimental results of comparative example 5 and example 6 show that by changing the type of the edible wax, certain temperature-sensitive characteristics can be given to the edible wax modified starch nanocrystalline particles, so that the release of the flavor components in the stable pickering emulsion can be controlled. Therefore, the Pickering emulsion can be used as a safe and effective flavor component sustained and controlled release system, a specific release temperature is given to the system through selection of edible waxes with different melting points, different types of emulsified products can be designed according to the temperature requirement during processing of a food system, and the Pickering emulsion has a good application prospect in the aspect of food additives.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. The food-grade temperature-sensitive pickering emulsion is characterized by comprising the following components in percentage by mass: 0.1-10% of edible wax modified starch nanocrystal, 10-60% of flavor components and the balance of water.
2. The food-grade temperature-sensitive pickering emulsion as claimed in claim 1, wherein the edible wax modified starch nanocrystal is prepared by the following steps: dissolving edible wax, stirring, adding the starch nanocrystal, stirring, mixing, reacting, adding deionized water with the same temperature as a reaction system, flushing the starch nanocrystal into an ice water bath of the system, collecting a sample, centrifuging, drying a precipitate in vacuum, grinding and crushing to finally obtain the starch nanocrystal with the hydrophobically modified surface, namely the wax modified starch nanocrystal.
3. The food-grade temperature-sensitive pickering emulsion as claimed in claim 2, wherein the starch nanocrystals are prepared by hydrolyzing native starch granules with concentrated sulfuric acid, wherein the native starch granules are one or more of waxy corn starch, common corn starch, tapioca starch, potato starch, rice starch or wheat starch.
4. The food-grade temperature-sensitive pickering emulsion according to claim 1, wherein the edible wax is one or more of paraffin wax, beeswax, carnauba wax, ozokerite, Chinese wax, rice bran wax, sunflower wax or lacquer wax.
5. The food grade temperature-sensitive pickering emulsion of claim 1, wherein the paraffin grade is at least one of 52, 54, 56, 58, 60, 62, 64, or 66.
6. The food-grade temperature-sensitive pickering emulsion according to claim 1, wherein the flavor component is one or more of beta-ionone, beta-citral, beta-pinene, citral, eugenol and peach aldehyde.
7. A preparation method of the food-grade temperature-sensitive Pickering emulsion as claimed in any one of claims 1 to 6, characterized in that the preparation method comprises the following steps: mixing the edible wax modified starch nanocrystal, the flavor components and water to obtain a mixed solution, then dispersing at a high speed, and dispersing the mixed solution by combining high-pressure homogenization or high-pressure microjet to prepare the temperature-sensitive Pickering emulsion.
8. The method according to claim 7, wherein the high speed dispersion is performed at 10000-22000 rpm for 2-5 min.
9. The method according to claim 7, wherein the high-pressure homogenization is performed at a pressure of 30 to 150MPa for 3 to 10 times.
10. The preparation method according to claim 7, wherein the pressure of the high-pressure micro-jet is 30-100 MPa, and the number of micro-jets is 2-5.
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