CN111961559B - Sterilizing and clarifying method of aged litchi alcoholic beverage - Google Patents
Sterilizing and clarifying method of aged litchi alcoholic beverage Download PDFInfo
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Abstract
The invention discloses a sterilization and clarification method of an aged litchi alcoholic beverage, which relates to the field of sterilization, purification, clarification and aging of alcoholic beverages and comprises the following steps: (1) litchi treatment, (2) litchi juice sterilization treatment: adding sucrose and malic acid into the litchi juice, adjusting sugar degree and pH, and adding dimethyl dicarbonate for normal temperature treatment to obtain sterilized litchi juice; (3) litchi juice fermentation: uniformly mixing the sterilized litchi juice, saccharomycetes, citric acid, amino acid, a preservative, vitamins and absolute ethyl alcohol, and sealing and fermenting to obtain a litchi alcoholic beverage; (4) the litchi alcoholic beverage clarification method comprises the following steps: adding bentonite into the litchi wine base, stirring, standing, collecting supernatant, and filtering to obtain clear wine; (5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-7 to 0 ℃, and preserving heat for 5-15 days to obtain the aged litchi alcoholic beverage.
Description
Technical Field
The invention relates to the field of sterilization, purification, clarification and aging of alcoholic beverages, in particular to a sterilization and clarification method of an aged litchi alcoholic beverage.
Background
China is a world where litchi fruits are produced, the litchi planting area and the litchi yield all account for the first world, the litchi is delicious in taste and rich in nutrition and is a very good fruit, however, fresh litchi is easy to deteriorate in the storage process, the storage cost is high, the litchi is not suitable for being preserved in the production period, and the rotting and deterioration of a large amount of litchi leads to the serious reduction of income of fruit growers, so that how to deeply process the litchi is to further improve the additional value of the litchi on the one hand, and on the other hand, the litchi which cannot be sold is treated to improve the income of the fruit growers has a very important meaning, and the litchi fruit wine production is a very good choice. The litchi fruit wine has faint scent, pleasant alcoholic strength and rich nutrient substances, and is popular with consumers.
The main component of the volatile acid is acetic acid which is a byproduct in the fermentation process, the concentration of the volatile acid plays a decisive role in the quality of the wine, and due to the existence of various mixed bacteria in litchi and the influence of relevant process formulas in the fermentation process, the acetic acid content of the litchi fruit wine is extremely easy to exceed the standard of 1.1g/L in the current litchi fruit wine industry in the production process of the litchi fruit wine.
CN201610357149.4 discloses a litchi fruit wine and a preparation method thereof, wherein the preparation method comprises the following steps: s1, mechanically crushing the drained litchi peels and seeds, and pulping the pulp into juice in a pulping machine; adding sucrose with the mass percent concentration of 15-30%, and adjusting the pH value to 3.3-3.8; s2, pouring the processed fruit juice and the crushed litchi rind and seed into a clean jar, leaving a 10-30% gap on the jar surface, and adding a potassium metabisulfite solution into the jar; s3, adding 1-10% of activated yeast liquid by mass into the fermentation liquor, carrying out aerobic fermentation for 12-24h at 20-28 ℃, then carrying out water sealing, and carrying out anaerobic fermentation for 8-12 days; s4, filtering the fermented supernatant with diatomite to obtain clear wine. The litchi fruit wine provided by the invention is mellow in taste, harmonious in litchi fruit aroma and bouquet, reddish in color, simple in preparation method, low in cost and capable of greatly improving the use value and economic benefit of litchi, and the condition that the common litchi fruit wine is yellowish and single in appearance quality is improved.
CN201210123096.1 discloses a method for preparing a low-alcohol litchi fruit wine beverage, which comprises the steps of juicing litchi pulp, crushing litchi shells, mixing with litchi juice, adding wine yeast, fermenting at low temperature until the alcoholic strength is 2-6%, centrifuging, filtering, homogenizing, sterilizing and canning to obtain the low-alcohol litchi fruit wine beverage. The litchi fruit wine is fermented at low temperature for a short time without adding exogenous sugar, the fermentation period is short, and the brewed litchi fruit wine has low alcoholic strength, moderate sour and sweet taste, fragrant fruit flavor, mellow mouthfeel and rich nutrition. The preparation method has simple process and short production period, and is suitable for industrial application.
CN201710636935.2 discloses a litchi fruit wine brewing method by adopting microwave radiation, which comprises the following steps: (1) pretreatment of litchi, (2) juice preparation, (3) fermentation; (4) aging: clarifying and purifying the fermented fruit juice to obtain litchi fruit wine; carrying out microwave irradiation treatment on the litchi fruit wine; ageing the fruit wine subjected to microwave irradiation at 10-0 ℃ for 1-3 months, blending, sterilizing, and sequentially freezing and packaging to obtain a product; the microwave irradiation treatment method is characterized in that microwave radiation is adopted for 30-60 s every day, and the treatment time is 1 month; the microwave condition is that the microwave frequency is 350MHz and the microwave power is 450W. The invention carries out microwave radiation treatment on the fermented fruit wine, provides reaction energy for substance reaction in the fruit wine, can promote the generation of esters and alcohol compounds in the fruit wine, improves the mellow fragrance and litchi fragrance of the fruit wine, and shortens the aging time.
In the prior art, sodium sulfite is added to kill infectious microbes in the fermentation broth, so that the volatile acid content of final fermentation is reduced, but the addition of sodium sulfite is harmful to human health and affects product sale; in the prior art, a microwave heating lamp mode is adopted for sterilization, so that harmful substances are not introduced, but effective components in the wine are damaged, and the quality of the wine is influenced. Therefore, how to adopt a better method to reduce the volatile acid content of the litchi fruit wine so as to improve the quality of the wine has very important social value.
Disclosure of Invention
The invention provides a sterilization and clarification method of an aged litchi alcoholic beverage, and the aged litchi alcoholic beverage obtained by the method is low in residual sugar content, complete in fermentation, low in volatile acid content, proper in alcoholic strength and mellow and normal in taste.
A sterilization and clarification method of an aged litchi alcoholic beverage is characterized by comprising the following steps: the following are all parts by mass,
(1) litchi treatment: selecting 5000 parts of nine-ripe fresh litchi fruits which are uniform in color and luster, good in form and free of diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi fruits in the mixed solution for 30-60min to remove harmful substances, then washing the litchi fruits clean with clear water, peeling, removing cores and pulping the litchi fruits, adding 100-plus 400mg of immobilized enzyme, uniformly mixing the immobilized enzyme and the immobilized enzyme while performing ultrasonic enzymolysis, wherein the ultrasonic power is 50-90w, the enzymolysis temperature is 18-26 ℃, the enzymolysis time is 1-4h, then squeezing the litchi fruits, filtering the litchi fruits by using a 100-plus 200-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 20-30obrix, the PH value is 3.8, then 1-1.5g of dimethyl dicarbonate is added, and the mixture is treated at normal temperature for 3-6 hours to obtain sterilized litchi juice;
(3) litchi juice fermentation: sterilizing litchi juice 1000 parts, yeast 10-50 parts, citric acid 2-6 parts, amino acid 40-100mg, and amino acid 10-40x10-3Preservative, 10-60x10-3Mixing vitamin and 30-80 parts of anhydrous ethanol, sealing, adjusting temperature to 10-20 deg.C, and fermenting for 8-15 days to obtain the final productTo obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.2-1 part of bentonite and 20-50 parts of dihydrolauryl litchi shell fiber into the litchi wine base, stirring uniformly, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-7 to 0 ℃, and preserving heat for 5-15 days to obtain the aged litchi alcoholic beverage.
Preferably, the litchi in the step (1) is one or a combination of a plurality of fruits of veronica sibirica, glutinous rice cakes, Huai branches, Feizixiao and black leaves.
Preferably, the enzyme in step (1) is one or a combination of cellulase, polygalacturonase, pectinolytic enzyme and pectinesterase.
Preferably, the preparation method of the immobilized enzyme comprises the following steps:
according to the mass portion, 8-12 portions of bisphenol A epoxy resin and 100015-22 portions of PEG are uniformly mixed, the mixture is heated to 68-75 ℃ while being stirred, 2.1-3.4 portions of TETA are added after the solution is clear and transparent, the mixture is reacted for 15-40min, the mixture is transferred to a PTFE mold, the mixture is kept warm and continuously reacted for 2-5h to obtain a white product, and the white product is cooled and washed by deionized water to obtain an epoxy resin macroporous polymer; soaking the epoxy resin macroporous polymer in TEOS for 2-5h, filtering, adding 8-12 parts of liquid ammonia, reacting for 8-12h at 50-60 ℃, drying, and roasting in a muffle furnace at 500-; taking 1-4 parts of porous silica carrier, adding 100-200mL of 1-5g/mL enzyme solution, placing in a constant-temperature water bath shaking table at 30-45 ℃ for shaking for 10-15h at the rotating speed of 100-120r/min, filtering out the immobilized enzyme, washing with buffer solution until the protein content in the supernatant can not be detected, and drying in vacuum at 25-30 ℃ to obtain the immobilized enzyme.
Preferably, the yeast in the step (3) is one or a combination of more of saccharomyces cerevisiae, candida utilis, torulopsis delbrueckii, debarked yeast and zygosaccharomyces bailii.
Preferably, the amino acid in step (3) is one or a combination of glutamic acid, arginine, histidine, D-alanine, L-arginine, L-glutamine, valine, leucine and isoleucine.
Preferably, the preservative in the step (3) is one or a combination of potassium sorbate and sodium benzoate.
Preferably, the vitamin in step (3) is one or a combination of inositol, thiamine and vitamin B1.
The litchi shell fiber adsorbing material adopts dihydrolauryl litchi shell fibers as raw materials:
the preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
The fibrous component of the lychee shells is mainly cellulose, R represents the lychee shell fibers, and the partial reaction equation is shown in figure 2.
Step 2, the dihydrolauryl litchi shell fiber is subjected to copolymerization reaction of oleic acid esterified litchi shell fiber and dihydromyrcenol, and the preparation method comprises the following steps:
according to the mass parts, evenly mixing 80-100 parts of oleic acid esterified lychee shell fiber, 3-5 parts of dihydromyrcenol, 2000 parts of 1000-one sodium silicate, 1-4 parts of ammonium persulfate and 1-3 parts of gelatin, controlling the temperature to be 70-80 ℃, stirring for 3-5h, filtering, washing with water and drying to obtain the dihydromyrcianyl lychee shell fiber.
The partial reaction equation is schematically shown in FIG. 3.
Further:
the reaction mechanism of the cell wall enzymolysis process in the preparation of the aged litchi alcoholic beverage is schematically shown in figure 4.
PEG-1000 is polyethylene glycol 1000 monostearate; TETA is triethylene tetramine; TEOS is tetraethyl orthosilicate.
Compared with the prior art, the invention has the beneficial effects that:
1. biological enzyme is added into litchi pulp, and ultrasonic is combined to destroy litchi cell walls, so that the juice yield of litchi in the squeezing process is improved, and the yield of litchi wine is improved;
2. the litchi juice is sterilized at normal temperature by adding the dimethyl dicarbonate, so that the mixed bacteria in the litchi juice are eliminated, the content of acetic acid generated in the fermentation process is greatly reduced, the active ingredients in the litchi juice are not damaged, and meanwhile, the dimethyl dicarbonate can be automatically degraded to generate a small amount of methanol and carbon dioxide, so that the health of a human body is not harmed;
3. the amino acid is added into the litchi juice, so that the nutrition content of the litchi wine is increased, the generation of acetic acid in the fermentation process is inhibited, and the flavor of the wine is improved;
4. the dihydrolauryl litchi shell fiber is obtained by copolymerization of oleic acid esterified litchi shell fiber and dihydromyrcenol, and can adsorb volatile acid of litchi wine and reduce volatile acid content.
Drawings
FIG. 1 is a Fourier infrared spectrum of the immobilized enzyme prepared in example 1:
at 464cm-1An absorption peak of silica at 1070/784cm is present in the vicinity-1An absorption peak of silicon oxygen exists nearby, which indicates that silicon dioxide participates in the reaction; at 2924cm-1The expansion and contraction absorption peak of the hydrocarbon exists nearby and is 1682cm-1The absorption peak of the amide near the carbonyl group is 1300cm-1And a stretching absorption peak of a carbon-nitrogen single bond exists nearby, so that the cellulase participates in the reaction.
FIG. 2 is a schematic diagram of the preparation principle of dihydrolauryl litchi shell fiber.
FIG. 3 is a schematic diagram of the preparation principle of oleic acid esterified lychee shell fiber and dihydromyrcenol through copolymerization.
FIG. 4 is a schematic diagram of a part of reaction mechanism of cell wall enzymolysis process in preparation of an aged litchi alcoholic beverage.
Detailed Description
The raw materials used in the following examples are all commercially available products, and the examples are further illustrative of the present invention and do not limit the scope of the present invention;
the performance test methods are as follows:
1. and (3) measuring the juice yield of the litchi juice: weighing clear and transparent litchi juice obtained by juicing, and dividing the obtained mass by the mass of litchi pulp;
2. and (3) measuring the content of acetic acid: testing according to a testing method of the content of volatile acid in GB/T15038-94;
3. sugar content determination: testing was performed according to the direct titration method of the total sugars test methods in GB/T15038-94;
4. alcohol content: the test was carried out by the alcohol meter method.
Example 1
(1) Litchi treatment: selecting 5kg of nine-ripe fresh immortal fruit litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 60min to remove harmful substances, then washing the litchi clean with clear water, peeling, removing cores and pulping, adding 100mg of immobilized cellulase, uniformly mixing, performing ultrasonic and enzymatic hydrolysis at an ultrasonic power of 50w and an enzymatic hydrolysis temperature of 18 ℃ for 4h, then squeezing, filtering the mixture by using a 100-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 20obrix, the PH value is 3.8, then 1g of dimethyl dicarbonate is added, and the mixture is treated for 6 hours at normal temperature to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 10g of saccharomyces cerevisiae, 2g of citric acid, 40mg of glutamic acid, 10mg of potassium sorbate, 10mg of inositol and 30g of absolute ethyl alcohol, sealing, adjusting the temperature to 10 ℃, and fermenting for 15 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.2g of bentonite and 20g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-7 ℃, preserving heat for 15 days, and obtaining the aged litchi alcoholic beverage.
The preparation method of the immobilized enzyme comprises the following steps:
uniformly mixing 8.0g of bisphenol A epoxy resin and PEG-100018.0 g, heating to 70 ℃ while stirring, adding 2.4g of TETA after the solution is clear and transparent, reacting for 15min, transferring to a PTFE (polytetrafluoroethylene) mold, then keeping the temperature and continuing to react for 2.5h to obtain a white product, cooling, and washing with deionized water to obtain an epoxy resin macroporous polymer; soaking an epoxy resin macroporous polymer in TEOS for 3h, filtering, putting into a container containing ammonia water atmosphere, reacting for 12h at 50 ℃, drying, and roasting for 3h at 600 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 1g of porous silica carrier into 100mL of 1g/mL enzyme solution, placing the porous silica carrier in a constant-temperature water bath shaking table at 35 ℃ and shaking for 10h, wherein the rotating speed is 100r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and carrying out vacuum drying at 25 ℃ to obtain the immobilized enzyme.
The preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
according to the mass g, uniformly mixing 80g of oleic acid esterified lychee shell fibers, 3g of dihydromyrcenol, 1000g of water, 1g of ammonium persulfate and 1g of gelatin, controlling the temperature to be 70 ℃, stirring for 3 hours, filtering, washing with water and drying to obtain the dihydrolauryl lychee shell fibers.
The preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 50g of lychee shell fibers into 200g of oleoyl chloride according to the mass g, controlling the temperature to be 80 ℃, stirring for 2h, filtering, washing to be neutral, drying, grinding into powder of 50 meshes, and obtaining the oleic acid esterified lychee shell fibers.
The juice yield of the litchi juice is 75%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.55g/L, the sugar content is 7g/L, and the alcoholic strength is 10%.
Example 2
(1) Litchi treatment: selecting 5kg of nine-ripe fresh Nuomici litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 53.4min to remove harmful substances, then washing the litchi clean solution with clear water, peeling, removing cores, pulping, adding 142mg of immobilized polygalacturonase, uniformly mixing, carrying out ultrasonic enzymolysis at the ultrasonic power of 61.2w at the enzymolysis temperature of 19.4 ℃ for 3.2h, then squeezing, filtering by using a 120-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 21.6obrix, the PH value is 3.8, then 1.1g of dimethyl dicarbonate is added, and the mixture is treated at normal temperature for 5.7 hours to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 20.4g of Candida utilis, 2.5g of citric acid, 48.4mg of arginine, 16.6mg of sodium benzoate, 22mg of thiamine and 44g of absolute ethyl alcohol, sealing, adjusting the temperature to 11.6 ℃, and fermenting for 13.6 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.3g of bentonite and 25g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-6 ℃, preserving heat for 14 days, and obtaining the aged litchi alcoholic beverage.
The preparation method of the immobilized enzyme comprises the following steps:
according to the mass parts, 9 parts of bisphenol A epoxy resin and 16 parts of PEG-1000are uniformly mixed, the mixture is heated to 69 ℃ while stirring, 2.2 parts of TETA is added after the solution is clear and transparent, the reaction is carried out for 17min, the PTFE mold is transferred, then the heat preservation is carried out, the reaction is continued for 3h, a white product is obtained, the temperature is reduced, and the deionized water is used for washing, so that the epoxy resin macroporous polymer is obtained; soaking an epoxy resin macroporous polymer in TEOS for 3h, filtering, adding 9 parts of liquid ammonia, reacting for 9h at 52 ℃, drying, and roasting for 3h at 520 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 120mL of 2g/mL enzyme solution into 2 parts of porous silica carrier, placing the porous silica carrier in a constant-temperature water bath shaking table at 33 ℃ and shaking for 11 hours, wherein the rotating speed is 105r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and drying the immobilized enzyme in vacuum at 26 ℃ to obtain the immobilized enzyme.
The preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
according to the mass g, 84g of oleic acid esterified lychee shell fiber, 3.2g of dihydromyrcenol, 1200g of water, 1.2g of ammonium persulfate and 1.4g of gelatin are uniformly mixed, the temperature is controlled at 72 ℃, stirring is carried out for 3.5h, and filtering, washing and drying are carried out to obtain the dihydrolauryl lychee shell fiber.
The preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 53g of lychee shell fibers into 230g of oleoyl chloride according to the mass g, controlling the temperature at 82 ℃, stirring for 3h, filtering, washing to be neutral, drying, and grinding into powder of 50 meshes to obtain the oleic acid esterified lychee shell fibers.
The juice yield of the litchi juice is 77.4%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.4g/L, the sugar content is 6.3g/L, and the alcoholic strength is 10%.
Example 3
(1) Litchi treatment: selecting 5kg of nine-ripe fresh Huai-Zhi-Li litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 50.4min to remove harmful substances, then washing the litchi clean with clear water, peeling, removing cores, pulping, adding 172mg of immobilized pectinolytic enzyme, uniformly mixing, carrying out ultrasonic enzymolysis while carrying out ultrasonic treatment, wherein the ultrasonic power is 67.6w, the enzymolysis temperature is 20.3 ℃, and the enzymolysis time is 2.6h, then squeezing, filtering by using a 132-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 24.4obrix, the PH value is 3.8, then 1.1g of dimethyl dicarbonate is added, and the mixture is treated for 5.1 hours at normal temperature to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 26g of Torulopsis delbrueckii, 3.1g of citric acid, 65.2mg of histidine, 22mg of potassium sorbate, 36mg of vitamin B1 and 53g of absolute ethyl alcohol, sealing, adjusting the temperature to 12.8 ℃, and fermenting for 11.9 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.4g of bentonite and 30g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-5 ℃, preserving heat for 12.2 days, and obtaining the aged litchi alcoholic beverage.
The preparation method of the immobilized enzyme comprises the following steps:
according to the mass parts, 10 parts of bisphenol A epoxy resin and 100017 parts of PEG (polyethylene glycol) -are uniformly mixed, the mixture is heated to 69 ℃ while being stirred, 2.5 parts of TETA (Tetraacetic acid) is added after the solution is clear and transparent, the reaction is carried out for 22min, a PTFE (polytetrafluoroethylene) mold is transferred, the reaction is carried out for 4h continuously after heat preservation, a white product is obtained, and the white product is cooled and washed by deionized water to obtain an epoxy resin macroporous polymer; soaking an epoxy resin macroporous polymer in TEOS for 4h, filtering, adding 10 parts of liquid ammonia, reacting for 10h at 55 ℃, drying, and roasting for 4h at 5800 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 180mL of 3g/mL enzyme solution into 3 parts of porous silica carrier, placing the porous silica carrier in a constant-temperature water bath shaking table at 38 ℃, shaking for 14 hours at the rotating speed of 115r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and drying the immobilized enzyme in vacuum at 27 ℃ to obtain the immobilized enzyme.
The preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
according to the mass g, uniformly mixing 90g of oleic acid esterified lychee shell fibers, 3.5g of dihydromyrcenol, 1400g of water, 1.6g of ammonium persulfate and 1.5g of gelatin, controlling the temperature to be 73 ℃, stirring for 3.5h, filtering, washing with water and drying to obtain the dihydrolauryl lychee shell fibers.
The preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 57g of lychee shell fibers into 270g of oleoyl chloride according to the mass g, controlling the temperature to be 85 ℃, stirring for 3h, filtering, washing to be neutral, drying, grinding into powder of 60 meshes, and obtaining the oleic acid esterified lychee shell fibers.
The juice yield of the litchi juice is 78.4%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.3g/L, the sugar content is 5.3g/L, and the alcoholic strength is 11%.
Example 4
(1) Litchi treatment: selecting 5kg of nine-ripe fresh Feizixiao litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 42min to remove harmful substances, then washing the litchi clean solution with clear water, peeling, removing cores and pulping the litchi, adding 238mg of immobilized pectinesterase, uniformly mixing the materials, carrying out ultrasonic and enzymolysis at an ultrasonic power of 72.4w and an enzymolysis temperature of 22.2 ℃ for 1.8h, then squeezing the mixture, filtering the mixture by using a 148-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 26obrix, the PH value is 3.8, then 1.1g of dimethyl dicarbonate is added, and the mixture is treated at normal temperature for 4.6 hours to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 30.8g of heterodera dekkera, 3.8g of citric acid, 78.4 mgD-alanine, 28.6mg of sodium benzoate, 50mg of inositol and 67g of absolute ethyl alcohol, sealing, adjusting the temperature to 13.8 ℃, and fermenting for 10.5 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.5g of bentonite and 35g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to-4 ℃, preserving heat for 9.8 days, and obtaining the aged litchi alcoholic beverage.
The preparation method of the immobilized enzyme comprises the following steps:
according to the mass parts, 11 parts of bisphenol A epoxy resin and 100017 parts of PEG are uniformly mixed, the mixture is heated to 70 ℃ while being stirred, 2.9 parts of TETA is added after the solution is clear and transparent, the reaction is carried out for 35min, the mixture is transferred to a PTFE (polytetrafluoroethylene) die, the reaction is continued for 4h while the temperature is kept, a white product is obtained, and the white product is cooled and washed by deionized water to obtain an epoxy resin macroporous polymer; soaking an epoxy resin macroporous polymer in TEOS for 4h, filtering, adding 10 parts of liquid ammonia, reacting for 11h at 57 ℃, drying, and roasting for 4h at 600 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 180mL of 4g/mL enzyme solution into 3 parts of porous silica carrier, placing the porous silica carrier in a constant-temperature water bath shaking table at 45 ℃ and shaking for 14 hours at the rotating speed of 118r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and drying the immobilized enzyme in vacuum at 29 ℃ to obtain the immobilized enzyme.
The preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
according to the mass g, 92g of oleic acid esterified lychee shell fiber, 3.7g of dihydromyrcenol, 1700g of water, 3g of ammonium persulfate and 1.7g of gelatin are uniformly mixed, the temperature is controlled at 78 ℃, stirring is carried out for 4 hours, and the dihydrolauryl lychee shell fiber is obtained after filtering, washing and drying.
The preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 73g of lychee shell fibers into 280g of oleoyl chloride according to the mass g, controlling the temperature at 87 ℃, stirring for 4h, filtering, washing to be neutral, drying, and grinding into powder of 50 meshes to obtain the oleic acid esterified lychee shell fibers.
The juice yield of the litchi juice is 79.4%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.2g/L, the sugar content is 4.5g/L, and the alcoholic strength is 11%.
Example 5
(1) Litchi treatment: selecting 5kg of nine-ripe fresh Feizixiao litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 30min to remove harmful substances, then washing the litchi clean with clear water, peeling, removing cores and pulping, adding 400mg of immobilized cellulase, uniformly mixing, performing ultrasonic and enzymatic hydrolysis at the ultrasonic power of 90w and the enzymatic hydrolysis temperature of 26 ℃ for 1h, then squeezing, filtering the mixture by using a 200-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into fructus litchi juice, and adjusting sugar degree to 30obrix, the PH value is 3.8, then 1.5g of dimethyl dicarbonate is added, and the mixture is treated for 3 hours at normal temperature to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 50g of saccharomyces cerevisiae, 6g of citric acid, 100mg of L-glutamine, 40mg of sodium benzoate, 60mg of vitamin B1 and 80g of absolute ethyl alcohol, sealing, adjusting the temperature to 20 ℃, and fermenting for 8 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 1g of bentonite and 40g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clear wine liquid to 70 ℃, preserving heat for 10min, then quickly cooling to 0 ℃, and preserving heat for 5 days to obtain the aged litchi alcoholic beverage.
The preparation method of the immobilized enzyme comprises the following steps:
according to the mass parts, uniformly mixing 12 parts of bisphenol A epoxy resin and 22 parts of PEG-1000, heating to 75 ℃ while stirring, adding 3.4 parts of TETA after the solution is clear and transparent, reacting for 40min, transferring to a PTFE (polytetrafluoroethylene) mold, then keeping the temperature and continuing to react for 5h to obtain a white product, cooling, washing with deionized water to obtain an epoxy resin macroporous polymer; soaking an epoxy resin macroporous polymer in TEOS for 5h, filtering, adding 12 parts of liquid ammonia, reacting for 12h at 60 ℃, drying, and roasting for 5h at 700 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 200mL of 5g/mL enzyme solution into 4 parts of porous silica carrier, placing the porous silica carrier in a constant-temperature water bath shaking table at 45 ℃, shaking for 15 hours at the rotating speed of 120r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and drying the immobilized enzyme in vacuum at 30 ℃ to obtain the immobilized enzyme.
The preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
uniformly mixing 100g of oleic acid esterified lychee shell fibers, 5g of dihydromyrcenol, 2000g of water, 4g of ammonium persulfate and 3g of gelatin according to the mass g, controlling the temperature to be 80 ℃, stirring for 5 hours, filtering, washing with water and drying to obtain the dihydrolauryl lychee shell fibers.
The preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 80g of lychee shell fibers into 320g of oleoyl chloride according to the mass g, controlling the temperature to be 92 ℃, stirring for 5h, filtering, washing to be neutral, drying, grinding into powder of 70 meshes, and obtaining the oleic acid esterified lychee shell fibers.
The juice yield of the litchi juice is 85%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.25g/L, the sugar content is 3g/L, and the alcoholic strength is 12%.
Comparative example 1
Compared with example 1, the litchi juice extraction rate was 71% by adding cellulase without immobilization, and the obtained aged litchi alcoholic beverage had a volatile acid content of 0.66g/L, a sugar content of 11.4g/L, and an alcoholic strength of 7%.
Comparative example 2
Compared with the embodiment 1, the enzymolysis process is not carried out ultrasonically, the juice yield of the litchi juice is 70%, the volatile acid content of the obtained aged litchi alcoholic beverage is 0.68g/L, the sugar content is 9.3g/L, and the alcoholic strength is 8%.
Comparative example 3
Relative to example 1, the amount of dimethyl dicarbonate added was 0g, the litchi extraction yield was 74%, and the obtained aged litchi alcoholic beverage had a volatile acid content of 1.5g/L, a sugar content of 9g/L, and an alcoholic strength of 10%.
Comparative example 4
In comparison with example 1, the amount of L-glutamine added was 0g, the litchi extraction rate was 75%, and the aged litchi alcoholic beverage had a volatile acid content of 1.3g/L, a sugar content of 7g/L, and an alcohol content of 10%.
Comparative example 5
Relative to example 1, (4) clarification method of litchi alcoholic beverage: adding 1g of bentonite into the litchi wine base, stirring uniformly, standing for 24h, taking supernatant, and filtering to obtain clear wine. The aged litchi alcoholic beverage has the volatile acid content of 3.35g/L, the sugar content of 15g/L and the alcoholic strength of 10%.
Claims (2)
1. A sterilization and clarification method of an aged litchi alcoholic beverage is characterized by comprising the following steps:
(1) litchi treatment: selecting 5kg of nine-ripe fresh immortal fruit litchi with uniform color, good shape and no plant diseases and insect pests, preparing a mixed solution of sodium chloride, sodium carbonate, sodium bicarbonate and water according to a mass ratio of 5:5:5:1000, soaking the litchi in the mixed solution for 60min to remove harmful substances, then washing the litchi clean with clear water, peeling, removing cores and pulping, adding 100mg of immobilized cellulase, uniformly mixing, performing ultrasonic treatment with ultrasonic power of 50w while performing enzymolysis, wherein the enzymolysis temperature is 18 ℃, the enzymolysis time is 4h, then squeezing, filtering by using a 100-mesh screen to obtain clear litchi juice, and testing the juice yield;
(2) and (3) litchi juice sterilization treatment: adding sucrose and malic acid into litchi juice, adjusting sugar degree to 20obrix and pH to 3.8, adding 1g dimethyl dicarbonate, and treating at room temperature for 6 hr to obtain sterilized litchi juice;
(3) litchi juice fermentation: uniformly mixing 1kg of sterilized litchi juice, 10g of saccharomyces cerevisiae, 2g of citric acid, 40mg of glutamic acid, 10mg of potassium sorbate, 10mg of inositol and 30g of absolute ethyl alcohol, sealing, adjusting the temperature to 10 ℃, and fermenting for 15 days to obtain litchi alcoholic beverage;
(4) the litchi alcoholic beverage clarification method comprises the following steps: adding 0.2g of bentonite and 20g of dihydrolauryl litchi shell fiber into the litchi wine base, uniformly stirring, standing for 24h, taking supernatant, and filtering to obtain clear wine;
(5) the wine liquid ageing process comprises the following steps: heating the clarified wine to 70 deg.C, maintaining for 10min, rapidly cooling to-7 deg.C, and maintaining for 15 days to obtain an aged litchi alcoholic beverage;
the preparation method of the dihydrolauryl litchi shell fiber comprises the following steps:
uniformly mixing 80g of oleic acid esterified lychee shell fibers, 3g of dihydromyrcenol, 1000g of water, 1g of ammonium persulfate and 1g of gelatin, controlling the temperature to be 70 ℃, stirring for 3 hours, filtering, washing with water and drying to obtain dihydromyrcial lychee shell fibers;
the preparation method of the oleic acid esterified lychee shell fiber comprises the following steps:
adding 50g of lychee shell fibers into 200g of oleoyl chloride, controlling the temperature to be 80 ℃, stirring for 2h, filtering, washing to be neutral, drying, and grinding into powder of 50 meshes to obtain the oleic acid esterified lychee shell fibers.
2. The method according to claim 1, wherein the immobilized cellulase in step (1) is prepared by: uniformly mixing 8.0g of bisphenol A epoxy resin and PEG-100018.0 g, heating to 70 ℃ while stirring, adding 2.4g of TETA after the solution is clear and transparent, reacting for 15min, transferring to a PTFE (polytetrafluoroethylene) mold, then keeping the temperature and continuing to react for 2.5h to obtain a white product, cooling, and washing with deionized water to obtain an epoxy resin macroporous polymer; soaking an epoxy resin macroporous polymer in TEOS for 3h, filtering, putting into a container containing ammonia water atmosphere, reacting for 12h at 50 ℃, drying, and roasting for 3h at 600 ℃ in a muffle furnace to obtain porous silicon dioxide; adding 1g of porous silica carrier into 100mL of 1g/mL enzyme solution, placing the porous silica carrier in a constant-temperature water bath shaking table at 35 ℃ and shaking for 10h, wherein the rotating speed is 100r/min, filtering out the immobilized enzyme, washing the immobilized enzyme by using buffer solution until the protein content in the supernatant can not be detected, and carrying out vacuum drying at 25 ℃ to obtain the immobilized enzyme.
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