CN113142538B - Zero-calorie candy for improving sweet taste performance of mogrosides and preparation method thereof - Google Patents
Zero-calorie candy for improving sweet taste performance of mogrosides and preparation method thereof Download PDFInfo
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- CN113142538B CN113142538B CN202110410802.XA CN202110410802A CN113142538B CN 113142538 B CN113142538 B CN 113142538B CN 202110410802 A CN202110410802 A CN 202110410802A CN 113142538 B CN113142538 B CN 113142538B
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- mogroside
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- erythritol
- water
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- 235000009508 confectionery Nutrition 0.000 title claims abstract description 51
- 235000019605 sweet taste sensations Nutrition 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 105
- 229920005989 resin Polymers 0.000 claims abstract description 105
- 239000004386 Erythritol Substances 0.000 claims abstract description 93
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 claims abstract description 93
- 235000019414 erythritol Nutrition 0.000 claims abstract description 93
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 claims abstract description 93
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 70
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- 229930191869 mogroside IV Natural products 0.000 claims description 15
- OKGRRPCHOJYNKX-UHFFFAOYSA-N mogroside IV A Natural products C1CC2(C)C3CC=C(C(C(OC4C(C(O)C(O)C(COC5C(C(O)C(O)C(CO)O5)O)O4)O)CC4)(C)C)C4C3(C)C(O)CC2(C)C1C(C)CCC(C(C)(C)O)OC(C(C(O)C1O)O)OC1COC1OC(CO)C(O)C(O)C1O OKGRRPCHOJYNKX-UHFFFAOYSA-N 0.000 claims description 15
- WRPAFPPCKSYACJ-UHFFFAOYSA-N mogroside IV E Natural products C1CC2(C)C3CC=C(C(C(OC4C(C(O)C(O)C(COC5C(C(O)C(O)C(CO)O5)O)O4)O)CC4)(C)C)C4C3(C)C(O)CC2(C)C1C(C)CCC(C(C)(C)O)OC1OC(CO)C(O)C(O)C1OC1OC(CO)C(O)C(O)C1O WRPAFPPCKSYACJ-UHFFFAOYSA-N 0.000 claims description 15
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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
- A23L27/30—Artificial sweetening agents
- A23L27/33—Artificial sweetening agents containing sugars or derivatives
- A23L27/34—Sugar alcohols
-
- 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
- A23L27/30—Artificial sweetening agents
- A23L27/33—Artificial sweetening agents containing sugars or derivatives
- A23L27/36—Terpene glycosides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
- Medicinal Preparation (AREA)
- Seasonings (AREA)
Abstract
The invention relates to a zero-calorie sugar for improving the sweet taste performance of mogroside and a preparation method thereof, wherein the zero-calorie sugar comprises the following components in mass content: 0.1-3.0wt% of mogroside V,0.007-0.9wt% of other mogrosides, 94.00-99.90wt% of erythritol. The zero-calorie sugar is obtained by compounding a momordica grosvenori high-power sweetener and erythritol and granulating by boiling, wherein the momordica grosvenori high-power sweetener is obtained by taking momordica grosvenori glycoside as a raw material, sequentially passing through a polar macroporous adsorption resin column, a high specific surface activity macroporous adsorption resin column and a small Kong Fanxiang gel column, and physically refining. According to the invention, phenolic acid, pigment and bitter taste components in mogrosides are removed through a specific process, the relative proportion of main sweet saponin components in the mogrosides is regulated, and the relative content is further regulated through an erythritol compounding technology, so that the sweet performance of the mogrosides is synergistically improved, and the sweet performance of the mogrosides is remarkably improved.
Description
Technical Field
The invention relates to the technical field of plant extraction and separation and the field of sweetener compounding, in particular to zero-calorie sugar for improving the sweet taste performance of mogroside and a preparation method thereof.
Background
The invention mainly relates to mogroside and erythritol.
1. Mogroside
The mogroside is prepared from fresh mature fruit of Momordica grosvenori of Cucurbitaceae by saccharification, ripening, and extracting. The most common commercial mogroside is V50, and the content of mogroside V is about 50%. The main process comprises the steps of saccharification, post-ripening, crushing, water extraction, filtration, ceramic membrane microfiltration clarification, broad-spectrum macroporous adsorption resin chromatography, ion exchange resin decolorization, desalination, vacuum concentration, spray drying and the like of fresh momordica grosvenori. The mogroside is the variety with the best taste and closest to sucrose in all natural sweet substances, has the remarkable advantages of fresh sweet taste, high sweetness and low calorie of sucrose, does not change blood pressure and blood sugar, does not cause caries and obesity, is particularly suitable for people suffering from diabetes, hypertension and obesity and people not suitable for eating sugar, is an ideal sugar substitute for healthy people, has no lasting bitter taste and metallic taste of stevioside, has no bitter and sweet taste of rubusoside, and is therefore most easily accepted by all people, and the mogroside is a special feature; however, the drawbacks of sweetness properties such as taste sensation at the mouth, sweetness multiplier, sweetness duration, etc. of the commercial mogroside limit the widespread use of the luo han guo extract.
The mogroside is separated and purified, so that most of substances in the fresh fructus momordicae, such as glucose, fructose, protein, amino acid, flavone, pigment and the like, are removed, but partial acid phenols still remain, and particularly V50 products which are most common in the market and have wide application range still have certain defects in the aspect of sweet taste: (1) the slightly bitter taste at the entrance disappears for about 8 seconds; (2) The sweetness multiple is 160-200 times of that of sucrose, the dosage is not easy to control, and the sweet taste multiple is not suitable to be directly used as a sweet substitute; and (3) lasting sweetness for up to about 45 seconds. In contrast, sucrose taste is sweet in mouth, no bitter and astringent, about 2 seconds up to the sweetness peak, and about 5 seconds disappear, which is currently the most desirable sweet taste. Therefore, improving the sweet taste of mogrosides to make them approach to the taste of sucrose has been a technical problem that one skilled in the art would expect to solve.
Factors influencing taste and mouthfeel of mogrosides are various, and literature reports that bittering saponins, i.e. mogrosides IIE, III, and the like exist in the momordica grosvenori, 2 components are commonly existing in the momordica grosvenori harvested in winter, and are mixed into autumn fruits in the production process, so that the finished product mogrosides has slightly bitter taste in the mouth; the inventor of the application discovers in long-term scientific research and production practice that phenolic acid, pigment and the like existing in the fresh momordica grosvenori can influence the taste and the mouth feel of the momordica grosvenori sweet glycoside, and on the premise that the product does not contain bitter saponin, the pure white momordica grosvenori sweet glycoside has the best taste and mouth feel, namely the fresh and sweet taste of sucrose; the inventor of the application also discovers that foreign matters introduced by decolorization of the ion exchange resin in the production process can greatly influence the taste and the mouthfeel of mogrosides if the foreign matters are not completely removed, and although a desalting step exists in the production process of the mogrosides, some foreign matters are not clear and cannot be completely removed.
Therefore, phenolic acid, pigment, bitter taste components and foreign matters which are generated by decoloring ion exchange resin and have an undefined structure are removed from the mogroside, and the relative proportion of main sweet saponin components is regulated, so that the taste and taste of the mogroside are improved, the sweetness factor is reduced, the sweetness duration is shortened, the obtained mogroside has excellent taste and sucrose-like refreshing sweetness, reaches the sweetness factor suitable for direct use, the sweetness duration is close to that of sucrose, and a sweet substitute-luohan fructose which is easily accepted by consumers is a key of the mogroside to a terminal application product, and is a key technical problem which needs to be solved by the industrialization of the mogroside.
2. Erythritol
Erythritol is a natural substance that has been widely used as a bulk sweetener. It is a four-carbon sugar alcohol with a molecular formula of C 4 H 10 O 4 . The white crystal powder has the advantages of refreshing sweet taste, low liability to moisture absorption, stability at high temperature, stability in a wide pH range, mild cooling feeling when dissolved in mouth, and suitability for various foods.
1. Characteristics (1)
Erythritol is white crystal, has sweetness about 70% of that of sucrose, and has cool feel. Zero heat. Is soluble in water (37%, 25 ℃) and is not degraded by enzyme due to lower solubility (compared with sucrose), can only be discharged from blood to urine through kidney (easy to be absorbed by small intestine) and does not participate in sugar metabolism and blood sugar change, so the food is suitable for diabetics. No fermentation in colon, and no gastrointestinal discomfort. Does not cause dental caries. Erythritol has high stability: the product is very stable to acid and heat, has very high acid and alkali resistance, can not be decomposed or changed at 160 ℃, can not be subjected to Maillard reaction to change color, and is particularly suitable for food processing with strict color requirements. Erythritol has an endothermic effect when dissolved in water, has a heat absorption of only 97.4KJ/KG, has a higher heat absorption degree than glucose and sorbitol, and has a cool feel when eaten. Erythritol is easy to crystallize, but cannot absorb moisture in a 90% humidity environment, and is easy to crush to obtain a powdery product, so that the erythritol can be used for preventing food from deteriorating due to moisture absorption on the surface of the food.
2. Function of
(1) Zero heat: erythritol is the only one type of zero-calorie sugar alcohol. Because of the small molecular weight, the erythritol which is easy to be absorbed by human body can be fermented by microorganism when only a small amount of erythritol enters large intestine of human body. Most erythritol enters the blood circulation, but the human body lacks enzymes capable of metabolizing erythritol, so that erythritol entering the blood cannot be digested and degraded, and can only be excreted from urine through the kidneys. Thus, erythritol has the characteristic of low calorie and is a natural zero-calorie bulk sweetener.
(2) High tolerance: the tolerance of human body to erythritol is 0.8 g per kilogram of body weight, and is one of the highest tolerance in sugar alcohols. The main reason is that erythritol has small molecular weight and little absorption and is mainly discharged through urine, thereby avoiding diarrhea caused by hypertonic phenomenon and avoiding flatulence caused by intestinal bacterial fermentation.
(3) Caries resistance: bacteria of the oral army, in particular streptococcus golden, cannot utilize and ferment erythritol, so that acidic substances are not produced to cause damage to teeth, and caries change occurs to the teeth.
(4) Promote proliferation of bifidobacteria: the utilization condition of the erythritol by the in-situ bacteria shows that the erythritol has obvious proliferation effect on bifidobacteria in the intestinal tract.
At present, the domestic research on momordica grosvenori extracts, especially representative momordica grosvenori sweet glycosides is very much, and mainly relates to an extraction and separation process of the momordica grosvenori sweet glycosides; many studies on compound sweeteners added with mogrosides have been conducted, mainly by compounding mogrosides with sugar alcohols, other plant extracts, etc. into sweeteners with low sweetness factors. Literature and patent reports on improved sweetness properties of mogrosides have been developed mainly from two aspects: firstly, removing bitter taste accompanied by mogroside; secondly, sweet fillers such as sugar alcohol and the like are added to dilute the bad taste. In the prior art, fresh momordica grosvenori is used as a starting material, the aim is to separate and prepare high-purity mogroside, or various types of simple compound are adopted, no commercial mogroside V50 is used as the starting material, phenolic acid, pigment, bitter and astringent ingredients in the mogroside and foreign matters generated by decoloring ion exchange resin are removed through a process technology, the relative proportion of main sweet saponin ingredients is regulated, and the pure-white mogroside with good taste is obtained, the V content of the mogroside is 55-70%, and the compound substances are added to synergistically improve the taste of the mogroside, so that the sweetness duration is shortened, and the taste is 1-10 times of that of sucrose; and reporting that the sweetness duration is less than or equal to 10 seconds.
The technical content and the solution related to improving the sweet taste performance of mogrosides disclosed in the prior art are as follows:
1. removing bitter taste associated with mogrosides.
CN201811397385.4 discloses a method for separating mogroside V from fructus momordicae, which comprises pulping fructus momordicae with water, sequentially carrying out plant enzyme enzymolysis and biological enzyme enzymolysis, collecting enzymolysis liquid, inactivating enzyme, fermenting, purifying with compound anion-cation exchange resin, concentrating and drying to obtain mogroside V. The product obtained by the preparation method is white, has no bitter taste, less solvent residue, no pesticide residue, stable product quality, and the obtained mogroside V is more than 60% and the total glycoside is more than 90%.
The method only uses anion-cation exchange resin for purification, only uses chemical exchange adsorption, does not have a special macroporous adsorption resin step, cannot obtain the snow white momordica grosvenori sweet glycoside, and has a certain amount of phenolic acid residues; foreign matter remains, and no purported bitter taste can not be achieved; the technology can not make the mogroside V more than 60%.
CN201711064166.X discloses a purification method of flavor mogroside V, comprising the following steps: (1) Polyamide adsorption: dissolving the crude extract of the mogroside with water, loading the solution on a polyamide resin chromatographic column, and collecting effluent; (2) alkali adjustment and ultrafiltration: regulating the pH value of the effluent liquid to 8-10, standing, coarse filtering, ultrafiltering and collecting filtrate; (3) ion exchange adsorption: sequentially loading the filtrate on a cation exchange resin column and an anion exchange resin column, and collecting effluent; (4) decoloring and drying: and (3) introducing the effluent into a decolorizing resin column, collecting the effluent, concentrating, and spray-drying to obtain the flavor mogroside V. In the product obtained by the method, the mass content of mogroside V is more than 60%, the yield is more than or equal to 90%, the mass content of the after-bitter source substance is less than 0.06%, the removal rate is more than 99.5%, the product has no after-bitter taste, fresh and cool mouthfeel, pure taste, good uniformity and stable property; the method is simple, has strong operability and is suitable for industrialized production.
The method adopts anion-cation exchange resin for purification and decolorizes with decolorizing resin, the basic principle is that foreign substances are introduced and remain, bitter and astringent ingredients cannot be thoroughly removed, the relative proportion of main sweet saponins cannot be regulated, and the method is possible to have no afterbitter taste, but the bitter taste of the mouth is still obvious and cannot be removed, and the optimal sweet ingredient proportion cannot be achieved.
CN201610860141.X discloses an extraction method of mogrosides without bitter taste, comprising the following steps: 1) Dissolving mogroside in water, adding DM130 macroporous resin, eluting with water to colorless, eluting with ethanol, collecting ethanol eluate, and recovering ethanol from eluate to obtain extract; 2) Dissolving the extract in water, adding D101+ macroporous resin, eluting with water, collecting eluate, concentrating, and drying. Compared with the prior art, the mogroside extracted by the invention does not contain bitter substances, and has pure sweet taste and no bitter taste.
The method is only refined by using broad-spectrum macroporous adsorption resin, and the 2 resins have strong adsorption capacity to mogrosides, flavone, pigment and the like, can not realize separation, can not remove phenolic acid substances in mogroside, can not be decolorized, and can not adjust the relative proportion of main sweet saponins.
CN201610860168.9 discloses a preparation method of debitterized momordica grosvenori extract, which comprises the following steps: 1) Extracting fructus Siraitiae Grosvenorii with ethanol, filtering the extractive solution, and recovering ethanol from the filtrate to obtain extract A; 2) Dissolving extract A in water, adding AB-8 macroporous resin, eluting with water to colorless, eluting with ethanol, collecting ethanol eluate, and recovering ethanol from eluate to obtain extract B; 3) Dissolving extract B in water, adding D101+ macroporous resin, eluting with water, collecting eluate, concentrating, and drying. Compared with the prior art, the momordica grosvenori extract prepared by the method does not contain bitter substances, and has pure sweet taste and no bitter taste.
The method is only refined by using broad-spectrum macroporous adsorption resin, and the 2 resins have strong adsorption capacity to mogrosides, flavone, pigment and the like, can not realize separation, can not remove phenolic acid substances in mogroside, can not be decolorized, and can not adjust the relative proportion of main sweet saponins.
CN200710003364.5 discloses a method for preparing decolored and debitterized momordica grosvenori extract, which is characterized in that: filtering the extractive solution with water as solvent, concentrating, decolorizing with decolorizing resin, eluting with ethanol, removing odor with deodorant, recovering ethanol, concentrating, spray drying, and pulverizing to obtain white and crystalline powder with no traditional Chinese medicine taste or bitter taste, wherein mogroside weight content is above 90%.
The method only uses decolorizing resin for refining, and 90% mogroside V can not be prepared; and the decolorized resin is eluted by ethanol, so that all components are eluted together, and the refining step is not actually carried out, wherein in practice, mogroside is not adsorbed by the decolorized resin in an exchange way and flows out in the feeding process, and pigment is adsorbed by the decolorized resin in an exchange way, and the ethanol eluting part is the components such as pigment, impurities and the like. The method can not debitterize the mogroside.
2. Adding sweet filler such as sugar alcohol to dilute the bad taste.
CN202010579810.2 discloses a sweet composition capable of replacing sucrose and a preparation method thereof, and the food additive composition comprises the following raw materials in parts by weight: 0.01-20 parts of special mixed powder; 0.01-40% of special xylitol; 25-99.96 parts of erythritol; l-arabinose 0.01-5; 0.01-10% of mogroside; the special mixed powder is as follows: 2-5 parts of papaya, 6-12 parts of coix seed, 3-12 parts of konjak, 2-5 parts of perilla, 1-3 parts of hawthorn, 3-12 parts of rhizoma polygonati, 4-8 parts of mulberry leaf, 4-8 parts of platycodon grandiflorum, 2-5 parts of medlar, 6-12 parts of cassia seed, 1-3 parts of lophatherum gracile, 2-4 parts of chrysanthemum and 2-8 parts of liquorice.
CN201910623559.2 discloses a sweet granule edible for diabetics and a preparation method thereof, wherein the sweet granule comprises the following raw materials in parts by weight: 0.1-0.5 part of Siraitia grosvenorii extract, 0.3-0.8 part of Litsea pungens extract, 60-80 parts of konjak fine powder and 10-30 parts of arabinose; the content of mogroside V in the fructus Siraitiae Grosvenorii extract is not less than 90%, the content of the lithocarpus litsea in the extract is 30-40% by weight of phlorizin and 60-70% by weight of trefoil glycoside, and the content of glucomannan in the konjak fine powder is more than 90%.
CN201711165148.0 discloses a method for preparing a compound sweetener, which has soft front taste, clean rear taste, no foreign taste and similar taste to sucrose. The product is characterized in that trehalose, arabinose (component A), mogroside, L-glycine and derivatives thereof (component B) and other natural sweet taste (component C) are uniformly mixed according to a certain formula proportion, or are dissolved in water according to a formula proportion, and then concentrated, crystallized or spray-dried to prepare the product.
The application of the compound sweetener related to the mogroside is that sugar alcohol, arabinose and the like are added on the basis of the mogroside, and one or more substances are prepared by simple processes, such as mixing, drying, granulating, drying and the like, and the compound sweetener only relates to simple proportion and does not relate to improving the taste and the mouthfeel of the mogroside from the technical aspect.
The technology and compounding method for improving the sweet taste performance of mogrosides are not ideal, and are particularly shown in the following: (1) The chemical exchange adsorption of ion exchange resin is used as a key for separation and purification, foreign substances are introduced, and the final product has residues, has no corresponding removal step or incomplete desalination, and causes the bitter taste of the mogroside product; (2) The broad-spectrum macroporous adsorption resin is used as the key of separation and purification, and the mogroside, phenolic acid, pigment and bitter and astringent ingredients are adsorbed and desorbed together, so that the mogroside and the phenolic acid, pigment and bitter and astringent ingredients cannot be effectively separated, and the taste is not improved; (3) The pure white mogrosides without phenolic acid, pigment and bitter taste cannot be prepared by the separation and purification technology of broad-spectrum macroporous adsorption resin and ion exchange resin, and the taste and the mouth feel of the current commercial mogrosides are all white to white, and the market proves that the taste and the mouth feel are still further improved; (4) The process technology for adjusting the relative proportion of the main sweet saponin components is not available, so that the optimal relative proportion of the main sweet saponin components cannot be maintained, and the most palatable feeling can be obtained through the synergistic effect; (5) The low-power sweet substance is compounded by adding sugar alcohol, arabinose and the like, only the simple proportioning is adopted, the sweetness and the bitter taste are simply diluted, only the quantity of each sweet component is changed, the taste and the mouth feel of the mogroside are not improved from the aspect of the object basis, the sweet performance advantage of the mogroside cannot be highlighted, and the taste and the mouth feel are still to be further improved.
The applicant prepares a high-power sweetener for improving the taste and the mouthfeel of mogroside in the prior patent application CN202110264251.0 and a preparation method thereof, can effectively remove the impurities affecting the mouthfeel such as acid phenol, pigment and the like, improves the mouthfeel of a mogroside high-power sweetener product, shortens the duration of sweetness, and simultaneously has no loss of an active ingredient mogroside V basically. Compared with the high-purity mogrosides in the market as the sweetener, the taste and the mouthfeel are obviously improved. However, the sweetness performance, particularly the aftersweetness, is still serious. However, the high-intensity sweetener still has long sweetness duration, and the taste and flavor of the high-intensity sweetener are improved compared with those of the conventional high-purity mogroside sweetener on the market, but the high-intensity sweetener is not satisfactory. Moreover, the high-power sweetener is inconvenient to use, has a sweetness multiple of 220-300 times, and can be directly used after being diluted by a large multiple when being used, and has low cost, but is popular in the market at present, the sweetness multiple is close to that of sucrose, and the sweetener can be directly eaten in a mode similar to that of sucrose, and is favored by common consumers in actual sales despite high product overflow. Therefore, there is a great commercial prospect in developing a low-intensity sweetener that can be used directly.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects, and provides the zero calorie sugar for improving the sweet taste performance of the mogroside and the preparation method thereof, wherein the market mogroside V50 specification is taken as a raw material, and ion exchange resin refining which is difficult to completely remove by introducing foreign substances and has influence on taste is not needed, but a pure physical adsorption separation purification method is adopted to remove phenolic acid, pigment and bitter taste components existing in the mogroside and foreign impurities and other unidentified substances generated by decoloring the ion exchange resin in the traditional process, and the main sweet saponins such as mogroside IV, mogroside V, 11-O-mogroside V, siamenoside I and mogroside VI are regulated by the process technology and the food additives with certain biological activity and sweet taste performance, so that the components reach the optimal taste proportion, thereby obviously improving the sweet taste performance of the mogroside, and preparing the mogroside which has excellent taste, fresh sweet taste and no bitter taste like sucrose and has 1-10 times of the sweetness; and the sweet duration is less than or equal to 10 seconds. The main factors of the sweetness times and the sweetness duration of the mogrosides are determined by the inherent physicochemical properties of the mogrosides, because the mogrosides belong to the saponins substances with natural triterpenes and high sweetness. However, the sweetness times and the sweetness duration are influenced by impurities which are caused by decolorization of some phenolic acids, pigments and ion exchange resins in the grosvenor momordica fruit and are associated with the mogroside and other substances with undefined structures, and on the other hand, the sweetness times and the sweetness duration of the mogroside can be obviously improved by the synergistic effect of the two substances. According to the invention, the special-treated mogroside high-power sweetener and erythritol are compounded, and the low-power compound mogroside zero-calorie candy is finally obtained through a boiling granulation process, so that the duration of sweetness can be greatly reduced, the taste and the taste are close to those of sucrose, and meanwhile, the flowability of the mogroside powder is improved through boiling granulation together with the erythritol, so that hardening is reduced. The Han fructose compound zero-calorie sugar provided by the invention is an ideal low-power sweetener for replacing sucrose.
The aim of the invention is achieved by the following technical scheme:
the zero-calorie candy for improving the sweet taste performance of the mogroside is characterized by comprising the following components in percentage by mass: 0.1-3.0wt% of mogroside V,0.007-0.9wt% of other mogrosides, 94.00-99.90wt% of erythritol.
The other mogrosides include mogroside IV, 11-O-mogroside V, siamenoside I, and mogroside VI.
Further, the zero-calorie sugar for improving the sweet taste performance of mogroside comprises the following components in mass content: 0.1-2.0wt% of mogroside V,0.02-0.35wt% of other mogrosides, 97.00-99.90wt% of erythritol; still further, the zero-calorie sugar for improving the sweet taste performance of mogroside comprises the following components in mass content: 0.13-0.93wt% of mogroside V,0.02-0.15wt% of other mogrosides, and 99.71-98.53wt% of erythritol.
In the zero calorie sugar, the mass content of the mogroside V is 5-7 times of that of other mogrosides; preferably, the mass content of mogroside V is 6-6.5 times of that of other mogrosides.
Further, the zero-calorie sugar for improving the sweet taste performance of the mogroside is obtained by compounding a high-power sweetener of the momordica grosvenori and erythritol and granulating by boiling, wherein the high-power sweetener of the momordica grosvenori is obtained by sequentially passing through a polar macroporous adsorption resin column, a high specific surface activity macroporous adsorption resin column, a small Kong Fanxiang gel column and a physical refining.
The solid of the Lo Han Guo high-intensity sweetener after being dried comprises the following components: 55 to 70 weight percent of mogroside V,1.5 to 4 weight percent of mogroside IV,3 to 10 weight percent of 11-O-mogroside V,0.5 to 1.8 weight percent of siamenoside, 0.4 to 1.5 weight percent of mogroside VI, less than 0.2 weight percent of acid phenolic substance and less than 0.2 weight percent of pigment substance; when the high intensity sweetener is a concentrate, the above ingredients and amounts thereof refer to the ingredients and amounts of the product obtained after drying (e.g., vacuum drying, spray drying, freeze drying) the concentrate, which is substantially free of moisture.
Preferably, the solid of the Lo Han Guo high-intensity sweetener after drying comprises the following components: 2.3 to 3.0 weight percent of mogroside IV,58 to 65 weight percent of mogroside V,5 to 7 weight percent of 11-O-mogroside V,0.9 to 1.3 weight percent of siamenoside, 0.7 to 1.1 weight percent of mogroside VI, less than 0.15 weight percent of acid phenolic substances and less than 0.1 weight percent of pigment substances.
The Lo Han Guo high intensity sweetener may be in the form of a solid (powder, granules, chunks), or in the form of a concentrate. So long as the solid (moisture less than or equal to 2%) of the Lo Han Guo high-power sweetener after drying has the components with the mass content.
The mogroside is preferably mogroside V50, wherein the mogroside V content is 42-55% of the specification, and is conventional commercially available product or powder of fructus Siraitiae Grosvenorii extract obtained by conventional method.
The acid phenol substances are fructus Siraitiae Grosvenorii polyphenol, kaempferol, amino acid, and phenolic acid with unknown structure. Due to the preparation process, especially in the sweetener which is obtained by adopting ion exchange resin and takes mogroside V as a main sweet component, especially in the product of mogroside V50 which is most common in the market, the partial acid phenol accounts for 2-5wt% of the mogroside, and the taste of the high-power sweetener which takes mogroside V as a main sweet substance is seriously influenced.
The polar macroporous adsorption resin is selected from at least one of ADS-7, LX-8, LX-17 and LX-38; the high specific surface activity macroporous adsorption resin is selected from at least one of LX-68G, XDA-7, XDA-200B, LX-10G, LSA-10 and LSA-5B; the small Kong Fanxiang GEL column has a particle size of 75-150 μm, and is one or two of polystyrene type (such as GEL CHP 20SS and GEL CHP 2 MG) or methacrylate type (such as GEL CHP 20SS and GEL CHP 2 MG).
Preferably, the high specific surface activity macroporous adsorption resin is modified by a cross-linking agent after chloromethylation, wherein the cross-linking agent is selected from polyamine; more preferably, the polyamine is at least one selected from ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, and polyethyleneimine. The amount of the cross-linking agent is 8-15wt% of the macroporous adsorption resin with high specific surface activity.
The specific modification method is that chloromethylated macroporous adsorption resin with high specific surface activity is added with a swelling agent for swelling, a catalyst and polyamine cross-linking agent are added, the temperature is raised, the stirring reaction is carried out for 10 to 20 hours, filtration, washing and drying are carried out, and the cross-linked modified macroporous adsorption resin with high specific surface activity is obtained.
The swelling agent is selected from nitrobenzene, dimethyl sulfoxide, toluene, and methylene chloride, and dimethyl sulfoxide is preferable as the swelling agent for toxicity. The swelling time is not 8-12h. Too long or too short swelling time is unfavorable for crosslinking modification of the macroporous adsorption resin with high specific surface activity.
Chloromethylation of macroporous adsorption resin is well known in the art, specifically, macroporous adsorption resin is added into carbon tetrachloride solution of 1, 4-dichloro methoxybutane, anhydrous zinc chloride is added after static swelling, stirring is carried out for 12-18h at 50-60 ℃, ethanol and deionized water are used for washing until no precipitate is added into silver nitrate solution, and chloromethylation of macroporous adsorption resin is completed.
The macroporous adsorption resin with high specific surface activity modified by the cross-linking agent reduces the pore canal of the resin, the specific surface area is further increased, pigment and phenolic acid molecules are easier to enter the pore canal, the molecular weight of saponins is relatively larger, and the saponins are not easy to diffuse in the pore canal of the resin, so that better separation can be realized. After the high specific surface active macroporous adsorption resin is crosslinked, the saturated adsorption rate of the mogroside is only 2-3%, so that the saponin can be ensured not to be lost basically.
The inventor finds that the conventional mogroside V50 product in the market contains a certain amount of phenolic acid, such as mogroside, kaempferol, amino acid, phenolic acid of an unknown structure and the like, and also contains partial pigment, particularly the V50 specification obtained by ion exchange resin, and has some unknown components due to the limitations of the extraction process and the production cost; the total amount of the phenolic acid in the momordica grosvenori product is about 2-5wt% due to different varieties and maturity of the momordica grosvenori and different processing technologies, and the total amount of the phenolic acid is not too much, but is a main factor affecting the taste of the momordica grosvenori sweet V50, and meanwhile, the pigment not only affects the color of the product, but also has a certain effect on the taste. Therefore, the invention adopts a physical adsorption mode without introducing other impurities, and uses polar macroporous adsorption resin and high specific surface activity macroporous adsorption resin to specifically and selectively adsorb phenolic acid and pigment. The inventor also discovers that the modified macroporous adsorption resin with high specific surface activity not only can effectively remove phenolic acid in the raw material, but also can not adsorb the mogroside V which is the main component. The economy of the method is ensured. Because the loss of mogroside V is not reimbursed if the impurities such as phenolic acid are finally removed. Therefore, the main technical problem to be solved by the invention is to remove impurities, improve the taste of mogroside V50 and reduce the loss of mogroside V as much as possible.
The high-power sweetener of the momordica grosvenori obtained by the specific method removes most of acid phenol and other impurities in the high-power sweetener, improves the taste of the mogroside, is compounded with erythritol to obtain the momordica grosvenori zero-calorie sugar through boiling granulation, the sweetness duration is further reduced by less than or equal to 10 seconds, and the momordica grosvenori zero-calorie sugar obtained through boiling granulation is a crystal with good fluidity, is not easy to absorb moisture, and can be stored for a long time without influencing the taste. Is a zero-calorie sugar which is suitable for being directly sold on the market and replaces sucrose.
The invention also provides a preparation method of the zero-calorie sugar for improving the sweet taste performance of the mogroside, which comprises the following steps:
(1) Preparing mogroside powder into mogroside water solution, passing through polar macroporous adsorption resin column, feeding, washing with purified water, and collecting feed effluent and water washing solution;
(2) Passing the combined effluent and water washing liquid in the step (1) through a macroporous adsorption resin column with high specific surface activity, feeding, washing the resin column with purified water, and collecting the feeding effluent and water washing liquid.
(3) Passing the combined effluent and water wash from step (2) through a small Kong Fanxiang gel column, collecting the feed effluent; after feeding, washing the gel column with water to obtain a small Kong Fanxiang gel column, and collecting the washing liquid; gradient eluting with alcohol-water mixed solution, and collecting high-concentration alcohol-water eluent; mixing the feed effluent, the water washing liquid and the high-concentration alcohol water eluting liquid, and vacuum decompressing until no alcohol smell exists to obtain refined liquid;
(4) Passing the refined solution obtained in the step (3) through a physical adsorption chromatographic column, feeding and washing with water, and combining the feeding effluent and the washing liquid;
(5) Concentrating the combined solution of the feeding effluent liquid and the water washing liquid in the step (4) under vacuum and decompressing to obtain concentrated solution, compounding the concentrated solution and erythritol, and granulating by boiling to obtain the product of the zero-calorie sugar for improving the sweet taste performance of the mogroside.
Preferably, in the step (1), the mogroside refers to a commercial mogroside V50 specification, wherein the content of the mogroside V is 42.0-55.0%, and the color is off-white to milk powder white; preparing a mogroside powder aqueous solution to obtain an aqueous solution with a solid content of 3-8 Brix.
Preferably, in the step (1), the addition amount of the polar macroporous adsorption resin is 5-10 times of the weight of the mogroside; the addition amount of the high specific surface active resin in the step (2) is 1 to 3 times of the weight of the mogroside; the addition amount of the small Kong Fanxiang gel in the step (3) is 15-30 times of the weight of the mogroside.
Preferably, in the step (1) and the step (2), the collecting part is a feed effluent and a water washing liquid, and the adding amount of the water washing liquid is 1-2 times of the mass of the polar macroporous adsorption resin and the high specific surface active macroporous adsorption resin respectively; in the step (3), the water consumption of the gel column with the water washing size of Kong Fanxiang is 1.5-2.5 times of that of the gel with the water washing size of Kong Fanxiang, and the use amount of the alcohol-water mixed solvent in the gradient elution of the alcohol-water mixed solvent is 2.5-4 times of that of the gel with the water washing size of Kong Fanxiang. The lower alcohol is at least one of methanol, ethanol and propanol, preferably ethanol.
Preferably, the macroporous adsorption resin with high specific surface activity in the step (2) is subjected to crosslinking modification. In the step (2), pure water is used for column feeding and elution, and the pure water has no desorption effect on mogrosides, so that certain loss of the mogrosides can be caused. After the high specific surface activity macroporous adsorption resin is subjected to crosslinking modification, on one hand, the adsorption of the paracetamol impurities can be enhanced, on the other hand, the yield of mogrosides can be improved, and the loss rate of the mogrosides can be reduced.
More preferably, the gradient elution in the step (3) is that the low-concentration alcohol-water mixed solvent with the volume concentration of 5-10% is used for eluting, and then the high-concentration alcohol-water mixed solvent with the volume concentration of 40-60% is used for eluting; further preferably, the volume ratio of the low-concentration alcohol-water mixed solvent to the high-concentration alcohol-water mixed solvent is 1-2:1-2. Preferably 1:1-1.2.
Preferably, in the step (4), the physical adsorption chromatographic column filler is one or any combination of granular activated carbon and chinlon activated carbon; the addition amount of the active carbon chromatographic column filler is 0.5-1.5 times of the weight of the mogroside V50; the dosage of the water washing water is 3-6 times of the weight of the mogroside.
Preferably, in step (5), the conditions of vacuum concentration under reduced pressure are well known in the art, and in one embodiment of the present invention, the vacuum concentration is performed under reduced pressure at a temperature of 60-65℃under a vacuum of-0.05 to-0.1 MPa. Concentrating under reduced pressure and vacuum to 20-25% solids content.
The boiling granulation process in the step (5) is that erythritol is put into a fluidized bed, the fluidized bed is kept in a boiling state, the heated and concentrated solution containing mogroside is taken as spraying liquid, the mixture is uniformly mixed, the boiling granulation is carried out to obtain crystals, and the product of the zero-calorie sugar for improving the sweetness performance of the mogroside is obtained.
The spraying liquid is concentrated liquid, preferably, the spraying liquid is prepared by compounding concentrated liquid and part of erythritol, and the rest erythritol is put into a fluidized bed. Preferably, the erythritol used in the spray-in with the concentrate formulation comprises 3-8%, preferably 4-6% of the total erythritol; the ratio of the concentrate to erythritol is not particularly limited as long as it satisfies that the content of mogroside V in the final product momordica grosvenori zero calorie sugar is in the range of 0.1 to 2.0wt%, and preferably, the ratio of the concentrate to erythritol is such that the content of mogroside V in the final product momordica grosvenori zero calorie sugar is in the range of 0.13 to 0.93wt%.
The process parameters for ebullating granulation are well known in the art. In one embodiment of the invention, the boiling granulation process conditions are a temperature of 70-75 ℃ and an injection rate of 7-10kg/h of the injection liquid.
Preferably, in step (5), the product of the dried concentrate, i.e. the Lo Han Guo high-intensity sweetener, mainly comprises the following components: 55 to 70 weight percent of mogroside V,1.5 to 4 weight percent of mogroside IV,3 to 10 weight percent of 11-O-mogroside V,0.5 to 1.8 weight percent of siamenoside, 0.4 to 1.5 weight percent of mogroside VI, less than 0.2 weight percent of acid phenolic substance and less than 0.2 weight percent of pigment substance; preferably, the Lo Han Guo high intensity sweetener comprises the following ingredients: 2.3 to 3.0 weight percent of mogroside IV,58 to 65 weight percent of mogroside V,5 to 7 weight percent of 11-O-mogroside V,0.9 to 1.3 weight percent of siamenoside, 0.7 to 1.1 weight percent of mogroside VI, less than 0.15 weight percent of acid phenolic substances and less than 0.1 weight percent of pigment substances.
The invention adopts a pure physical adsorption separation purification method, does not introduce foreign impurities, and has remarkable effect. The macroporous adsorption resin is used in a combination mode according to a certain sequence, so that most of phenolic acid, pigment and other impurities in the mogroside product are removed, and the mogroside is basically not adsorbed, so that separation is realized, the taste is improved, the main component mogroside V is basically not lost, and the retention rate is more than 90%; the small Kong Fanxiang gel has a molecular separation function, can perform primary separation on substances with different molecular weights and molecular structures, has a certain adsorption on phenolic acid, pigment and foreign substances and mogroside components generated by decolorization of the original process ion exchange resin, can realize separation of mogroside and the impurities from the molecular structures and the molecular weights by combining water washing in a gradient elution mode through aqueous ethanol with different concentrations, and can regulate the composition of main saponin sweet components, so that the taste and mouthfeel of the mogroside are obviously improved; the active carbon chromatography can adsorb phenolic acid, pigment, foreign substances, peculiar smell and the like generated by decolorization of the ion exchange resin in the prior art, basically has no adsorption to mogrosides, and can clarify the pure-taste mogroside solution in a simple way. Through the combination of the above technologies, phenolic acid, pigment and bitter and astringent ingredients in mogroside and foreign impurities generated by decolorizing with ion exchange resin in the traditional process are removed, the relative proportion of main saponin sweet ingredients is regulated, and the sweet property of mogroside is improved from the technical aspect. The pure mogroside prepared by the process technology has higher content of key index component, i.e. mogroside V, and 220-280 times of sucrose sweetness, and the sweetness performance is not optimal at the moment. The applicant finds that the bulk sweetener, erythritol, has a synergistic effect with pure mogroside, has the effects of obviously improving the taste of mogroside, reducing sweetness multiple, shortening the duration of sweetness and simultaneously has the effect of caries resistance, and is free of calories, so that the sweetness performance and the biological activity of mogroside are fully exerted. The relative contents of main sweet components in mogrosides, such as mogroside IV, mogroside V, 11-O-mogroside V, siamenoside I and mogroside VI, are further regulated by erythritol, so that the optimum taste proportion of the components can be achieved, and the sweet performance of the mogroside is further improved from the aspect of a new compound thought.
The pure mogroside is powder, has poor fluidity and certain hygroscopicity. Through boiling granulation, the powder form of the mogroside can be changed, the fluidity is improved, the hardening is reduced, and the mogroside is dried, so that the mogroside zero-calorie candy with improved sweetness performance of the mogroside is prepared. In a preferred boiling granulating process, a small amount of erythritol and a concentrated solution containing mogroside, from which most of acid phenol, pigment and other impurities are removed, are processed together to prepare an injection solution, so that the injection solution contains a certain amount of erythritol, and the momordica grosvenori zero-calorie sugar obtained by boiling granulating is more uniform and stable in product quality, namely a product with higher mogroside content, has low moisture absorption rate, ensures the storage stability of the product, and is more beneficial to consumers.
The invention has the beneficial effects that:
(1) The invention provides a method for improving the sweet taste performance of mogroside. Phenolic acid, pigment, bitter taste components and foreign substances introduced by decolorization of ion exchange resin in a product of the commercial mogroside V are removed by a specific process, the relative proportion of main sweet saponin components in the mogroside is regulated, the relative content is further regulated by an erythritol compounding technology, and the sweet performance of the mogroside is synergistically improved by synergy, so that the sweet performance of the mogroside is remarkably improved.
(2) According to the invention, the main sweet saponin components in the mogroside, namely the relative proportions of mogroside IV, mogroside V, 11-O-mogroside V, siamenoside I and mogroside VI, are regulated by special resin according to a specific separation and purification sequence, so that the taste and mouthfeel of the mogroside are obviously improved.
(3) The method provides a key technology of pure physical separation and purification to replace ion exchange resin decolorization chemical exchange adsorption, solves the problem that the decolorization effect cannot be achieved by secondary ion exchange resin decolorization under the conditions of no foreign substances and chemical exchange reaction, and prepares pure white momordica grosvenori zero-calorie sugar.
(4) In the preferred technical scheme of the invention, through crosslinking modification of the macroporous adsorption resin with high specific surface activity, resin pore channels are reduced, meanwhile, the specific surface area is further increased, pigment and phenolic acid molecules enter the pore channels more easily, and the molecular weight of saponins is relatively larger and is not easy to diffuse in the resin pore channels, so that better separation can be realized, and meanwhile, the retention rate of mogroside V is further increased.
(5) The boiling granulating method of the invention improves the fluidity of the momordica grosvenori sweet glycoside powder and reduces hardening. The erythritol is divided into two parts, a small amount of erythritol and a concentrated solution are prepared into spraying liquid, and then the spraying liquid and the rest erythritol are boiled and granulated together, so that a product with more uniform and stable quality is obtained, and even a product with higher mogroside V content can keep not to absorb moisture for a long time, so that the product is convenient for consumers to purchase and use.
(6) The invention provides a sweetener for improving the sweet taste performance of mogroside, namely Lo Han Guo zero-calorie sugar. The main sweet components are as follows: 0.1-2.0wt% of mogroside V,0.02-0.35wt% of other mogrosides, 97.00-99.90wt% of erythritol; the color is pure white, and the property is crystallization; the sweetness is 1-10 times of that of sucrose; the sweet taste duration is less than or equal to 10 seconds; sweetness performance: the cane sugar is fresh and cool, has pure sweet taste, no bitter taste, good taste and good mouthfeel, and is basically the same as the cane sugar.
Detailed Description
The invention is further illustrated below with reference to examples.
The mogroside V50 used in the embodiment of the invention is produced by Hunan Hua Cheng biological resource Co., ltd, and is prepared by the following steps: the method comprises the steps of saccharification, post-maturation, crushing, water extraction, filtration, ceramic membrane microfiltration clarification, broad-spectrum macroporous adsorption resin chromatography, ion exchange resin decolorization, desalination, vacuum concentration, spray drying and the like of fresh momordica grosvenori to obtain the momordica grosvenori extractive solution, wherein the momordica grosvenori extractive solution comprises 3.72% of mogroside IV, 51.62% of mogroside V, 5.96% of 11-O-mogroside V, 0.95% of siamenoside I and 0.92% of mogroside VI; 3.25% of total amount of Momordica polyphenol, kaempferol, amino acid, phenolic acid with unknown structure, etc. (measured by UV method).
Erythritol was purchased from bowling organism stock, inc; the purified water is prepared by a secondary pure water device for production workshops, and the macroporous adsorption resin Kong Fanxiang gel, the activated carbon filler for chromatography and the raw and auxiliary materials are all obtained by conventional commercial paths if no special description exists.
In the embodiment of the invention, the taste and the sweetness multiple and the sweetness duration are measured by using the perception; the mogroside IV, mogroside V, 11-O-mogroside V, siamenoside I, and mogroside VI content is determined by High Performance Liquid Chromatography (HPLC), the phenolic acid content is determined by Fu Lin Fenfa, and the absorbance at 765nm is measured by ultraviolet-visible spectrophotometry (UV).
Preparation example 1 crosslinking modification of XDA-200B resin
Adding 1kg of XDA-200B resin, 3.5L of BCMB,12L of carbon tetrachloride into a stirred reaction kettle, standing and swelling for 10h, adding 0.2kg of anhydrous zinc chloride, reacting for 12h under the stirring condition of 60 ℃, and washing with absolute ethyl alcohol and deionized water until no precipitate is generated when nitrate solution is added after the reaction is finished, thus obtaining chloromethylated XDA-200B resin. Adding chloromethylated XDA-200B resin into dehydrated 12L dimethyl sulfoxide to swell for 8 hours, slowly adding 0.2kg anhydrous aluminum chloride, 0.1kg anhydrous zinc chloride and 0.08kg triethylenetetramine, heating to 50 ℃ to react for 12 hours under stirring, filtering, washing with absolute ethanol and deionized water respectively until nitrate solution is added to generate no precipitate, placing the obtained resin into a blast dryer, and drying in vacuum at 60 ℃ overnight to obtain the crosslinked modified XDA-200B resin.
The pore size of the crosslinked modified XDA-200B resin was reduced from 150 to 90 by testing.
Preparation example 2 crosslinking modification of LSA-5B resin
Adding 1kg of LSA-5B resin, 3.5L of BCMB and 12L of carbon tetrachloride into a reaction kettle with stirring, standing and swelling for 10 hours, adding 0.2kg of anhydrous zinc chloride, reacting for 12 hours under the stirring condition of 60 ℃, and washing with absolute ethyl alcohol and deionized water until no precipitate is generated when nitrate solution is added after the reaction is finished, thus obtaining chloromethylated LSA-5B resin. Adding chloromethylated LSA-5B resin into dehydrated 12L dimethyl sulfoxide to swell for 8 hours, slowly adding 0.2kg anhydrous aluminum chloride, 0.1kg anhydrous zinc chloride and 0.12k ethylenediamine, heating to 50 ℃ to react for 12 hours under stirring, filtering, washing with absolute ethyl alcohol and deionized water respectively until nitrate solution is added and no sediment is generated, placing the obtained resin into a blast dryer, and drying in vacuum at 60 ℃ overnight to obtain the crosslinked modified LSA-5B resin.
The pore size of the crosslinked modified LSA-5B resin was tested to reduce from 130 angstroms to 80 angstroms.
Example 1
(1) 80kg of LX-17 resin is filled in a stainless steel chromatographic column in advance and is treated with ethanol, 4% sodium hydroxide aqueous solution and 4% hydrochloric acid according to a macroporous adsorption resin regeneration treatment standard procedure for standby. Taking 10kg of mogroside V50 powder, adding 150L of purified water, stirring for dissolution, and then passing the dissolution through a chromatographic column filled with LX-17 resin to collect feed effluent; after the feed was completed, a 130L purification water-washed resin column was further added, and the water-washed liquid was collected, and the feed effluent and the water-washed liquid were combined.
(2) 18kg of the crosslinked modified XDA-200B resin obtained in preparation example 1 was packed in a stainless steel column in advance and treated with ethanol, 4% aqueous sodium hydroxide solution and 4% hydrochloric acid according to a macroporous adsorbent resin regeneration standard procedure for use. Passing the combined solution obtained in the step (1) through a chromatographic column filled with XDA-200B resin, and collecting a feed effluent; after the completion of the feeding, the mixture was further fed into a 35L purification washing resin column, and the washing liquid was collected. The feed effluent and the water wash are combined.
(3) 200kg of GEL CHP 20SS filler is filled in a stainless steel chromatographic column in advance and treated with ethanol and purified water for later use. Passing the combined solution obtained in the step (2) through a chromatographic column filled with small Kong Fanxiang gel, and collecting feeding effluent to obtain feed liquid 1; after the feeding, 400L of purified water washing column is further fed, and water washing liquid is collected to obtain feed liquid 2.
Then ethanol-water solution gradient elution is carried out: advanced 300L of 8% ethanol-water solution with volume concentration, and the effluent is additionally collected; then 350L of 40% ethanol is added, and the eluent in the section is collected to obtain feed liquid 3.
Mixing the materials 1, 2 and 3 to obtain mixed solution, concentrating under reduced pressure at-0.085 MPa and 63 deg.C, recovering ethanol until no smell of alcohol, and concentrating to obtain refined solution.
(4) The stainless steel chromatographic column is filled with 9kg of granular active carbon for chromatography in advance and treated with ethanol and purified water for standby. Passing the refined solution through a chromatographic column filled with granular activated carbon, and collecting the feed effluent; after the feeding, the mixture was further fed into a 36L purified water washing column, and the water washing liquid was collected. Combining the feed effluent and the water washing liquid to obtain the pure-taste mogroside solution.
(5) Concentrating the pure mogroside solution under vacuum at 65 deg.C and vacuum degree-0.085 MPa to 20.1% solid content to obtain 37.0kg concentrate. Taking 4.4kg of erythritol, adding 20.0L of purified water, stirring, and dissolving to obtain erythritol solution; and then taking 1.0kg of concentrated solution, and stirring and uniformly mixing the concentrated solution and the erythritol solution to obtain a compound solution serving as spraying solution.
(6) Boiling and granulating. (1) Taking 95.4kg of erythritol, putting the erythritol into a fluidized bed, and keeping a boiling state and a medium-high wind speed at a temperature of 72 ℃; (2) spraying the compound liquid at a constant speed of 8.5kg per hour; (3) mixing well, drying to obtain 97.9kg crystal, which is Momordica grosvenori zero-calorie sugar.
According to detection, the concentrated solution obtained in the step (5) of the embodiment is dried to obtain a powdery product which is basically free of water, namely, in the high-power sweetener of momordica grosvenori, the content of mogroside IV is 2.51%, the content of mogroside V is 63.75%, the content of 11-O-mogroside V is 6.65%, the content of siamenoside I is 1.06% and the content of mogroside VI is 0.92%; the total amount of the polyphenol, kaempferol, amino acid and phenolic acid with unknown structure of the grosvenor momordica fruit is 0.04%, and the retention rate of the mogroside V is 93.35%. .
Through detection, the momordica grosvenori has good taste and basically the same as that of sucrose, and has no slight bitter taste; the sweetness is 1 time of that of sucrose; sweetness duration 7 seconds; mogroside V content is 0.13%, other mogrosides content is 0.02%, and erythritol content is 99.71%.
Example 2
(1) 100kg of ADS-7 resin is filled in a stainless steel chromatographic column in advance, and the mixture is treated with ethanol, 4% sodium hydroxide aqueous solution and 4% hydrochloric acid according to a macroporous adsorption resin regeneration treatment standard procedure for standby. Taking 10kg of mogroside V50 powder, adding 200kg of purified water, stirring for dissolution, and then passing the dissolution through a chromatographic column filled with ADS-7 resin to collect feed effluent; after the feeding, the resin column is washed with 180L of purified water, and the washing liquid is collected. The feed effluent and the water wash are combined.
(2) The crosslinked and modified LSA-5B resin obtained in preparation example 2 was put into a stainless steel chromatographic column in advance for 25kg and treated with ethanol, 4% sodium hydroxide aqueous solution and 4% hydrochloric acid according to the standard procedure of macroporous adsorption resin regeneration treatment for later use. Passing the combined solution obtained in the step (1) through a chromatographic column filled with LSA-5B resin, and collecting a feeding effluent; after the completion of the feeding, the resin column was further washed with 50L of purified water, and the washing solution was collected. The feed effluent and the water wash are combined.
(3) 240kg of methacrylate type GEL CHP 2MG filling material is filled in a stainless steel chromatographic column in advance, and ethanol and purified water are used for treatment. Passing the decolorized solution through a chromatographic column filled with small Kong Fanxiang gel, and collecting the feed effluent to obtain feed liquid 1; after the feeding, 500L of purified water is added into the column, and the water washing liquid is collected to obtain feed liquid 2.
Then gradient elution is carried out by using the aqueous ethanol: 400L of 7% ethanol is advanced, and the effluent is additionally collected; then 500L of 42% ethanol is added, and the eluent in the section is collected to obtain feed liquid 3.
Mixing the materials 1, 2 and 3 to obtain mixed solution, concentrating under reduced pressure at-0.085 MPa and 61 deg.C, recovering ethanol until no smell of alcohol, and concentrating to obtain refined solution.
(4) The stainless steel chromatographic column is filled with 12kg of chinlon activated carbon for chromatography in advance and treated with ethanol and purified water for standby. Passing 270L of refined solution through a chromatographic column filled with chinlon activated carbon, and collecting feed effluent; after the feeding, the mixture was further fed into a 50L purified water washing column, and the water washing liquid was collected. Combining the feed effluent and the water washing liquid to obtain the pure-taste mogroside solution.
(5) Compounding and adjusting the sweet taste performance; concentrating the mogroside solution under vacuum at-0.085 MPa and 62 deg.C to 22.6% solid content under reduced pressure to obtain 36.4kg concentrate. Taking 7.0kg of erythritol, adding 15.0L of purified water, stirring, and dissolving to obtain erythritol solution; and then taking 12.9kg of concentrated solution, and stirring and uniformly mixing the concentrated solution and the erythritol solution to obtain a compound solution serving as spraying solution.
(6) Boiling and granulating. (1) Taking 90.3kg of erythritol, putting the erythritol into a fluidized bed, and keeping a boiling state and a medium-high wind speed at a temperature of 75 ℃; (2) spraying the compound liquid at a constant speed of 9.0kg per hour; (3) mixing uniformly to obtain 98.3kg of crystal of the product momordica grosvenori zero-calorie sugar.
According to detection, the concentrated solution obtained in the step (5) of the embodiment is dried to obtain a powdery product which is basically free of water, namely the high-power sweetener of momordica grosvenori, wherein the content of mogroside IV is 2.36%, the content of mogroside V is 60.41%, the content of 11-O-mogroside V is 6.62%, the content of siamenoside I is 1.06% and the content of mogroside VI is 1.01%; the total amount of the momordica grosvenori polyphenol, kaempferol, amino acid, phenolic acid with unknown structure and the like is 0.07 percent, and the retention rate of the mogroside V is 92.18 percent.
Through detection, the momordica grosvenori has good taste and basically the same as that of sucrose, and has no slight bitter taste; the sweetness is about 11 times that of sucrose; the sweetness duration is 10 seconds; mogroside V content is 1.64%, other mogrosides content is 0.26%, erythritol content is 97.61%.
Example 3
The other operations and conditions were the same as in example 1 except that 37.0kg of the concentrate was obtained in step (5). Taking 5.0kg of erythritol, adding 20.0L of purified water, stirring, and dissolving to obtain erythritol solution; and then taking 7.4kg of concentrated solution, and stirring and uniformly mixing the concentrated solution and the erythritol solution to obtain a compound solution serving as spraying solution.
(6) Boiling and granulating. (1) Taking 92.5kg of erythritol, putting the erythritol into a fluidized bed, and keeping a boiling state and a medium-high wind speed at a temperature of 72 ℃; (2) spraying the compound liquid at a constant speed of 8.5kg per hour; (3) mixing uniformly to obtain 98.4kg of crystal of Siraitia grosvenorii zero-calorie sugar.
Through detection, the momordica grosvenori has good taste and basically the same as that of sucrose, and has no slight bitter taste; the sweetness is 7 times that of sucrose; the sweetness duration was 9 seconds; mogroside V content is 0.93%, other mogrosides content is 0.15%, erythritol content is 98.53%.
Example 4
Other operations and conditions were the same as in example 3 except that 7.4kg of the concentrated solution was taken as the injection solution in step (5);
(6) Boiling and granulating. (1) Taking 97.5kg of erythritol, putting the erythritol into a fluidized bed, and keeping a boiling state and a medium-high wind speed at a temperature of 72 ℃; (2) spraying the compound liquid at a constant speed of 8.5kg per hour; (3) mixing uniformly to obtain 98.4kg of crystal of Siraitia grosvenorii zero-calorie sugar.
Example 5
Other operations and conditions were the same as in example 2 except that 12.9kg of the concentrated solution was taken as the injection solution in step (5);
(6) Boiling and granulating. (1) Taking 97.3kg of erythritol, putting the erythritol into a fluidized bed, and keeping a boiling state and a medium-high wind speed at a temperature of 75 ℃; (2) spraying the compound liquid at a constant speed of 9.0kg per hour; (3) mixing uniformly to obtain 98.3kg of crystal of the product momordica grosvenori zero-calorie sugar.
Example 6
Other operations and conditions were the same as in example 1 except that the cross-linked modified XDA-200B resin in step (2) was replaced with an unmodified XDA-200B resin.
Through detection, the white powdery product of the high-power sweetener of momordica grosvenori obtained by drying the concentrated solution obtained in the step (5) has the content of 2.43 percent of mogroside IV, 61.84 percent of mogroside V, 5.45 percent of 11-O-mogroside V, 1.13 percent of siamenoside I and 0.95 percent of mogroside VI; the total amount of the momordica grosvenori polyphenol, kaempferol, amino acid, phenolic acid with unknown structure and the like is 0.15 percent, and the retention rate of the mogroside V is 88.93 percent.
The product momordica grosvenori zero-calorie sugar is obtained by final boiling granulation, and detected, the momordica grosvenori zero-calorie sugar obtained by the embodiment has good taste, is basically the same as sucrose, and has no slight bitter taste; the sweetness is about 1 time of that of sucrose; sweetness duration 7 seconds; mogroside V content is 0.126%, other mogrosides content is 0.022%, and erythritol content is 99.81%.
Comparative example 1
The V50 specification mogrosides produced by Hunan Huacheng biological resource Co., ltd are high-power sweeteners. I.e. the raw materials treated in the above examples of the invention.
Comparative example 2
(1) Taking 0.1kg of V50-specification mogroside produced by Hunan China Chengsheng biological resource Co., ltd as high-power sweetener, taking 1.8kg of erythritol, adding 20.0L of purified water, stirring, and dissolving to obtain a compound solution of V50 and erythritol as an injection solution;
(2) Boiling and granulating. (1) 39.8 kg of erythritol is taken and put into a fluidized bed, and the boiling state and the medium and high wind speed are kept at 72 ℃; (2) spraying the compound liquid at a constant speed of 8.5kg per hour; (3) mixing well, drying to obtain 40.4kg crystal, which is Momordica grosvenori zero-calorie sugar.
Through detection, the momordica grosvenori has good taste and basically the same as that of sucrose, and has no slight bitter taste; the sweetness is 1 time of that of sucrose; sweetness duration 7 seconds; mogroside V content is 0.12%, other mogrosides content is 0.02%, erythritol content is 99.58%.
Application example 1
The characteristics of the sweeteners obtained in the examples and comparative examples of the present invention were evaluated by using 20 blind tests, and the specific method is as follows:
1. screening and training of sensory analysts
Sensory panelists were screened according to the rules of GB/T16291.2-2010, and after taste sensitivity training, 20 sensory panelists (each half of men and women) were finally screened to make up a sensory panel.
2. Duration of sweetness: the test person was asked to taste the aqueous solution of the compound sweetener diluted to a sweetness close to 5wt% sucrose solution of the present invention. Starting from the time the panelist's consumption, the time at which the subject perceived sweetness disappeared was recorded, excluding data from those subjects who taste 5wt% sucrose sweetness duration deviated from 5 seconds by more than 1 second, i.e., excluding data from those subjects who taste 5wt% sucrose/brown sugar solution sweetness duration less than 4 seconds and greater than 6 seconds. The average value finally obtained is the duration of sweetness of the sweetener of the invention.
3. Subjective evaluation of taste:
sensory analysts restricted their diets, especially food consumption, within 1h before the start of the assessment experiment, which could severely affect taste. For different taste experiments, each group selects 12 most suitable sensory analysts from 20 to carry out sensory evaluation of the compound sweetener solution. The odor and taste of the sweetener solution are comprehensively scored and evaluated, the score is 1 to 10, 5 weight percent of sucrose is used as a reference, the satisfaction is highest, 10 is 10, each time the questionnaire tester is 12 people, the highest score is removed, the lowest score is removed, and finally the overall average value is calculated.
The test samples are divided into a product group and a control group, the product group is prepared by adding the Momordica grosvenori zero-calorie sugar obtained in the embodiment and the comparison example of the invention to be close to the sweetness of 5wt% of sucrose solution, 10mL of the solution to be evaluated is taken to be contained in a disposable paper cup, the solution is discharged after staying for a plurality of seconds by a sensory evaluation staff, the evaluation time interval is 20 minutes, and the evaluation result is an average value scored by 10 evaluation staff. The sensory evaluation criteria of the control group was 10 minutes full.
The test results are shown in table 1 below:
TABLE 1
As can be seen from the data in Table 1, according to the present invention, the impurities affecting the taste of the sweetener, such as the acid phenol, remained in the mogroside V50 product were effectively removed by a specific preparation process, and the mogroside V as a main component was not substantially lost, and the retention rate was substantially over 90%. Compounding the concentrated solution and erythritol, and granulating by boiling to obtain the momordica grosvenori zero-calorie sugar which is white crystal particles; the sweetness is 1-15 times of that of sucrose/brown sugar; sweetness duration is less than or equal to 10 seconds, sweetness performance: fresh and cool, pure sweet, no bitter taste, good taste and taste, and is basically the same as sucrose. The preparation method is simple and low in cost, can effectively improve the taste of the mogroside and enlarge the audience of the mogroside products.
In addition, by comparing examples 3 and 4 with examples 2 and 5, it can be seen whether all erythritol is fed as solid into the fluidized bed in the boiling granulation process, or a small amount of erythritol and a concentrated solution containing mogroside are compounded to be used as spraying liquid, and then the spraying liquid and other erythritol are boiled and granulated together, so that the taste and flavor of the final product momordica grosvenori zero calorie sugar are not influenced.
As can be seen from comparative example 1, the mogroside V50 provided by the invention has greatly improved sweetness performance as sweetener; comparative example 2 was a direct combination of untreated mogroside V50 with erythritol, and the obtained mogroside V content was similar to example 1, but the mouthfeel was far less than example 1, with a slightly bitter taste. The treatment process of the mogroside V50 is successful, the loss rate of the mogroside V is in an acceptable range while the taste is improved, but the taste is obviously improved, the product sales is facilitated, and the popularization of the mogroside in consumers is enlarged.
Application example 2
The grosvenor momordica zero calorie sugar of examples 1-6 was compared by visual inspection as follows: visual inspection of appearance was rated according to the following scale: class a: the granularity is consistent, the particles are spherical, and the fluidity is good; class B: the granularity has deviation which can be identified by naked eyes, is spherical, ellipsoidal and has general fluidity; class C: the particle size has obvious difference and shows various irregular shapes and poor fluidity.
The moisture content is evaluated by accurately weighing a certain mass (m 0 ) The sweeteners of examples and comparative examples were placed on a petri dish, placed in a 65RH% incubator at 25 ℃, removed after 12 hours, and tested for mass (m 1 ). Moisture regain (%) =m according to the following formula 1 -m 0 /m 0 X 100%. The results obtained are shown in Table 2 below:
TABLE 2
Momordica grosvenori zero calorie sugar | Appearance (visual inspection) | Moisture rate |
Example 1 | A | 2.17% |
Example 2 | A | 2.63% |
Example 3 | A | 2.54% |
Example 4 | A | 2.86% |
Example 5 | A | 5.24% |
Example 6 | A | 2.21% |
As can be seen from the data in Table 2, the momordica grosvenori zero-calorie sugar prepared by the embodiment of the invention has the advantages of uniform granularity, good fluidity and low moisture content. Moreover, by comparing the embodiment 3 with the embodiment 4 and comparing the embodiment 2 with the embodiment 5, it is believed that the use of adding a small amount of erythritol into the spraying liquid is more beneficial to the uniform stability of the product, especially for the product with higher mogroside content, the lower moisture content can be ensured, the market sales is facilitated, and the product overflow price is improved.
Claims (11)
1. The zero-calorie candy for improving the sweet taste performance of the mogroside is characterized by comprising the following components in percentage by mass: 0.1-3.0wt% of mogroside V,0.007-0.9wt% of other mogrosides, 94.00-99.90wt% of erythritol;
The preparation method of the zero-calorie sugar for improving the sweet taste performance of the mogroside comprises the following steps:
(1) Preparing mogroside powder into mogroside water solution, passing through polar macroporous adsorption resin column, feeding, washing with purified water, and collecting feed effluent and water washing solution;
(2) Passing the combined effluent and water washing liquid in the step (1) through a macroporous adsorption resin column with high specific surface activity, feeding, and then using a purified water washing resin column to collect the fed effluent and water washing liquid;
the high specific surface activity macroporous adsorption resin is prepared by modifying macroporous adsorption resin through a crosslinking agent after chloromethylation, wherein the chloromethylation of the macroporous adsorption resin is prepared by adding the macroporous adsorption resin into a carbon tetrachloride solution of 1, 4-dichloro methoxybutane, standing and swelling, adding anhydrous zinc chloride, stirring for 12-18h at 50-60 ℃, washing with ethanol and deionized water until no precipitate is formed when the silver nitrate solution is added, and finishing chloromethylation of the macroporous adsorption resin; swelling chloromethylated macroporous adsorption resin with swelling agent, adding catalyst and polyamine crosslinking agent, heating and stirring to react for 10-20h, filtering, washing, and drying to obtain crosslinked modified macroporous adsorption resin with high specific surface activity; the swelling agent is selected from nitrobenzene, dimethyl sulfoxide, toluene or methylene dichloride, and the swelling time is 8-12h; the cross-linking agent is at least one selected from ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine and polyethyleneimine; the dosage of the cross-linking agent is 8-15wt% of the high specific surface activity macroporous adsorption resin;
(3) Passing the combined effluent and water wash from step (2) through a small Kong Fanxiang gel column, collecting the feed effluent; after feeding, washing the gel column with water to obtain a small Kong Fanxiang gel column, and collecting the washing liquid; gradient eluting with alcohol-water mixed solution, and collecting high-concentration alcohol-water eluent; mixing the feed effluent, the water washing liquid and the high-concentration alcohol water eluting liquid, and vacuum decompressing until no alcohol smell exists to obtain refined liquid;
(4) Passing the refined solution obtained in the step (3) through a physical adsorption chromatographic column, feeding and washing with water, and combining the feeding effluent and the washing liquid;
(5) Concentrating the combined solution of the feeding effluent liquid and the water washing liquid in the step (4) under vacuum and decompressing to obtain concentrated solution, compounding the concentrated solution and erythritol, and granulating by boiling to obtain the zero-calorie sugar for improving the sweet taste performance of the mogroside;
in the step (5), the concentrated solution comprises the following components after being dried: 55-70 wt% of mogroside V, 1.5-4 wt% of mogroside IV, 3-10 wt% of 11-O-mogroside V,0.5-1.8wt% of siamenoside, 0.4-1.5 wt% of mogroside VI, less than 0.2wt% of acid phenolic substances and less than 0.2wt% of pigment substances.
2. The zero-calorie sugar according to claim 1, characterized by comprising the following components in mass content: 0.1-2.0wt% of mogroside V,0.02-0.35wt% of other mogrosides, 97.00-99.90wt% of erythritol.
3. The zero-calorie sugar according to claim 1, wherein the zero-calorie sugar comprises the following components in mass content: 0.13-0.93wt% of mogroside V,0.02-0.15wt% of other mogrosides, and 99.71-98.53wt% of erythritol.
4. The zero-calorie sugar according to claim 1, wherein in step (5), the concentrate, after drying, comprises the following components: 2.3-3.0wt% of mogroside IV, 58-65wt% of mogroside V, 5-7wt% of 11-O-mogroside V, 0.9-1.3wt% of siamenoside, 0.7-1.1wt% of mogroside VI, less than 0.15wt% of acid phenolic substances and less than 0.1wt% of pigment substances.
5. The zero-calorie sugar according to claim 1, wherein the polar macroporous adsorbent resin is selected from at least one of ADS-7, lx-8, lx-17, lx-38; the macroporous adsorption resin with high specific surface activity is selected from at least one of LX-68G, XDA-7, XDA-200B, LX-10G, LSA-10 and LSA-5B; the small Kong Fanxiang gel column has a particle size of 75-150 μm, and is one or two of polystyrene type and methacrylate type.
6. The zero-calorie sugar according to claim 1, wherein in the step (1), the mogroside powder is a commercially available mogroside V50 specification, wherein the mogroside V content is 42.0-55.0%; preparing a mogroside powder aqueous solution to obtain an aqueous solution with a solid content of 3-8 Brix; the addition amount of the polar macroporous adsorption resin is 5-10 times of the weight of the mogroside;
The addition amount of the high specific surface active resin in the step (2) is 1-3 times of the weight of the mogroside;
the addition amount of the small Kong Fanxiang gel in the step (3) is 15-30 times of the weight of the mogroside;
in the step (1) and the step (2), the addition amount of the water washing liquid is 1-2 times of the mass of the polar macroporous adsorption resin and the high specific surface active macroporous adsorption resin respectively;
in the step (3), the water consumption of the gel column with the water washing size of Kong Fanxiang is 1.5-2.5 times of that of the gel with the water washing size of Kong Fanxiang, and the use amount of the alcohol-water mixed solvent in the gradient elution of the alcohol-water mixed solvent is 2.5-4 times of that of the gel with the water washing size of Kong Fanxiang.
7. The zero-calorie sugar according to claim 1, wherein the gradient elution in step (3) is performed by eluting with a low concentration alcohol-water mixed solvent having a concentration of 5 to 10% by volume and then eluting with a high concentration alcohol-water mixed solvent having a concentration of 40 to 60% by volume.
8. The zero-calorie sugar according to claim 7, wherein the volume ratio of the low-concentration alcohol-water mixed solvent to the high-concentration alcohol-water mixed solvent is 1-2:1-2.
9. The zero-calorie sugar according to claim 1, wherein the boiling granulation process in the step (5) is that erythritol is put into a fluidized bed, the fluidized bed is kept in a boiling state, the mixture is heated, a concentrated solution containing mogroside is used as an injection liquid, the mixture is uniformly mixed, and the mixture is subjected to boiling granulation to obtain crystals, so that the zero-calorie sugar with the effect of improving the sweetness of the mogroside is obtained.
10. The zero-calorie sugar according to claim 9, wherein the injection is a combination of a concentrate and a portion of erythritol, and the remainder of erythritol is fed into the fluidized bed; erythritol used for preparing injection with the concentrated solution accounts for 3-8% of the total erythritol.
11. The zero-calorie sugar according to claim 10, characterized in that the erythritol used in the preparation of the spray with the concentrate comprises 4-6% of the total erythritol.
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