CN115477985A - Health-care rice wine and preparation method thereof - Google Patents
Health-care rice wine and preparation method thereof Download PDFInfo
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- CN115477985A CN115477985A CN202211267612.8A CN202211267612A CN115477985A CN 115477985 A CN115477985 A CN 115477985A CN 202211267612 A CN202211267612 A CN 202211267612A CN 115477985 A CN115477985 A CN 115477985A
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- 240000007651 Rubus glaucus Species 0.000 description 1
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Classifications
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Abstract
The invention discloses a preparation method of health-care rice wine, which comprises the following steps: mixing glutinous rice, cassava, rice, wheat and water, and steaming to obtain a fermented material; cooling the fermented material, mixing with the composite nutrient material, adding distiller's yeast and water, and fermenting to obtain crude wine; filtering the crude wine to obtain filtrate; sterilizing the filtrate with high-voltage pulse electric field to obtain health rice wine. The health-care rice wine disclosed by the invention is pleasant in flavor and unique in taste, and has good antioxidation and insomnia relieving effects.
Description
Technical Field
The invention belongs to the technical field of rice wine processing, and particularly relates to health-care rice wine and a preparation method thereof.
Background
The rice wine is mainly prepared from glutinous rice through processes of soaking, stewing, fermenting, filtering, sterilizing and the like, contains not only saccharides, polypeptides, amino acids, vitamins, mineral substances and the like, but also alcohol, ester, organic acid and other flavor components, has higher nutrition, and can promote blood circulation to remove blood stasis, warm kidney and strengthen yang and enhance immunity when being drunk in a proper amount. In the rice wine making process, the distiller's yeast is important to the quality and flavor of rice wine and determines the success or failure of wine making. Glutinous rice wine koji is commonly used for brewing wines with glutinous rice as a raw material. In addition, in order to improve and enrich the nutrition and taste of the traditional rice wine, it has been reported that the medicinal and edible raw materials with different efficacies are used in the brewing process of the rice wine, such as blueberry, black fungus, quinoa, medlar, raspberry and the like, and the rice wine is improved in aspects of color, aroma, taste and the like by coupling the raw materials with the brewing process of the rice wine.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides health-care rice wine and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a preparation method of health rice wine comprises the following steps:
a1, mixing sticky rice, cassava, rice, wheat and water according to a mass ratio of (0.5-1.5): (0.5-1.3): (0.4-1.6): 0.2-1.5): 5.5-10), and cooking at 95-100 ℃ for 45-70min to obtain a fermented material;
a2, cooling the fermentation material to 33-36 ℃, adding distiller's yeast and water, and fermenting for 63-75h to obtain crude wine; the mass ratio of the fermentation material to the distiller's yeast to the water is (3.5-5.5) to (0.5-1.5) to (10-20);
a3, filtering the crude wine to obtain a filtrate; sterilizing the filtrate at 63-67 deg.C with high-voltage pulse electric field to obtain health rice wine; the electric field intensity of the high-voltage pulse electric field is 48-52kV/cm, the pulse width is 380-430 mus, the pulse frequency is 8-12Hz, the pulse number is 4-24, and the processing time is 0.5-2s.
Preferably, the preparation method of the health-care rice wine comprises the following steps:
a1, mixing sticky rice, cassava, rice, wheat and water according to a mass ratio of (0.5-1.5): (0.5-1.3): (0.4-1.6): 0.2-1.5): 5.5-10), and cooking at 95-100 ℃ for 45-70min to obtain a fermented material;
a2, cooling the fermentation material to 33-36 ℃, uniformly mixing the fermentation material with the composite nutrient material, adding distiller's yeast and water, and fermenting for 63-75 hours to obtain crude wine; the mass ratio of the fermentation material to the distiller's yeast to the water is (3.5-5.5) to (0.5-1.5) to (10-20); the mass ratio of the composite nutrient material to the fermentation material is 1 (8-12);
a3, filtering the crude wine to obtain a filtrate; sterilizing the filtrate at 63-67 deg.C with high-voltage pulse electric field to obtain health rice wine; the electric field intensity of the high-voltage pulse electric field is 48-52kV/cm, the pulse width is 380-430 mus, the pulse frequency is 8-12Hz, the pulse number is 4-24, and the processing time is 0.5-2s.
The preparation method of the composite nutrient material comprises the following steps: washing rhizoma gastrodiae, poria cocos, liquorice, dried orange peel and mulberry with water, drying in the air, and crushing to 50-100 meshes to obtain mixed powder, wherein the mass ratio of the rhizoma gastrodiae to the poria cocos to the liquorice to the dried orange peel to the mulberry is (0.2-0.6) to (1-2); mixing the mixed powder with water according to the mass ratio of 1 (10-15), adding a compound enzyme for enzymolysis for 50-60min at 40-60 ℃ and 50-100rpm, wherein the mass ratio of the compound enzyme to the mixed powder is (1-5) to 100, and the compound enzyme is formed by mixing pectinase and cellulase according to the mass ratio of 1 (1-3); after the enzymolysis is finished, heating to 95-100 ℃ and keeping for 3-5min; cooling to room temperature, performing ultrasonic treatment at 20-30kHz and 200-350W for 10-30min, centrifuging, and collecting supernatant.
The distiller's yeast is prepared by the following method:
s1, mixing glutinous rice, cassava, rice and wheat according to a mass ratio of (1-5) to (1-5), drying at 45-55 ℃ for 0.5-2h, and then crushing and sieving with a 20-40-mesh sieve to obtain dry powder;
s2, mixing the dry powder and water according to a mass ratio of (0.7-1.3) to (2.5-4.2), stirring at a rotating speed of 25-35rpm for 2-4h at a temperature of 22-27 ℃, and simultaneously performing ultrasonic treatment with power of 320-350W and frequency of 38-42 kHz; then steaming and boiling for 40-48min at 90-110 ℃ to obtain cooked slurry;
s3, sterilizing the cooked slurry at 62-68 ℃ by using a high-voltage pulse electric field to obtain sterilized cooked slurry; the electric field intensity of the high-voltage pulse electric field is 48-52kV/cm, the pulse width is 380-420 mu s, the pulse frequency is 8-12Hz, the pulse number is 4-24, and the processing time is 0.5-2s;
s4, concentrating the sterilized cooked slurry for 0.8-2h at the temperature of 58-62 ℃ under the vacuum degree of 33-38kPa, and then cooling to 33-38 ℃ to obtain concentrated slurry;
s5, inoculating a fermentation strain into the concentrated slurry, adding glucose and the polygonum flaccidum extraction liquid, and fermenting for 14-20 days at the temperature of 33-38 ℃ and the relative humidity of 80-92% in a sterile environment to obtain the distiller' S yeast; the mass ratio of the fermentation strain, the concentrated slurry, the glucose and the polygonum hydropiper extract is (3-7): 90-115): 20-25): 4-7; the fermentation strain is a mixture of microzyme, aspergillus japonicus, mucor circinelloides, bacillus pumilus, soil glutamic acid bacillus and lactobacillus plantarum according to the mass ratio of (1-6) to (1-6).
The preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum herb at 42-48 ℃ for 0.5-2H, crushing, sieving with a 40-60-mesh sieve, adding water, decocting at 85-92 ℃ for 40-48min, and concentrating at 55-62 ℃ under the vacuum degree of 0.08-0.3kPa for 0.5-1.5H to obtain polygonum flaccidum herb concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 23-27 ℃ for 24-30H by using H2, and treating by using ultrasonic waves with power of 360-400W and frequency of 36-40kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 0.8-1.2mol/L, and the concentration of ethanol is 50-58wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is (1.8-3.2) to (0.7-1.3);
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 190-210cm, and the diameter of the chromatographic column is 16-19cm; the loading capacity of the modified glucan in the chromatographic column is 70-80% of the volume of the column body;
h4, loading the polygonum flaccidum concentrated solution into a chromatographic column at 30 ℃, collecting filtrate, and concentrating the filtrate for 1H at 55-65 ℃ under the vacuum degree of 0.08-0.2kPa to obtain polygonum flaccidum extract liquid, wherein the chromatographic flow rate is 170-190 mL/H.
The folk traditional method for promoting the production and fermentation of distiller's yeast by using polygonum hydropiper comprises the following steps: the addition of the polygonum hydropiper in the distiller's yeast can enhance the unique flavor of the rice wine, prevent rancidity and peculiar smell, promote the growth and reproduction activities of adopted zymophyte, improve the quality of the distiller's yeast and prolong the quality guarantee period of the rice wine. However, the polygonum hydropiper used in the traditional process contains anthraquinone, and the anthraquinone belongs to one of 2B carcinogen lists which are preliminarily collated and referred to by carcinogen lists published by international cancer research institutes of world health organization. Therefore, the invention aims to provide a process technology capable of reducing the content of anthraquinone in the polygonum hydropiper extract; furthermore, the reduction of anthraquinone can provide a better fermentation environment condition for the zymophyte, thereby producing the health rice wine with better quality.
The 6-amino nicotinic acid contains carboxyl and amino with stronger polarity, and the two groups have specific relative positions so as to have a specific electronegativity center; the relative position and spatial configuration of carbonyl and silicon in bis (trimethylsilyl) carbonyldiimine enable the bis (trimethylsilyl) carbonyldiimine to have polarity within a specific range, the combination of the two is used as a synergist to promote the long-chain structure of linoleic acid to be cross-linked with glucan molecules in a spiral winding manner, the spatial entanglement complexity of glucan is further improved, the number ratio of introduced carboxyl, amino, carbonyl and silicon can form specific electronegativity strength, the adsorption effect on anthraquinone in polygonum hydropiper concentrated solution is enhanced, and the residual amount of anthraquinone in the prepared polygonum hydropiper extract is reduced. When the modified glucan prepared by the invention is used for chromatography of the polygonum flaccidum concentrated solution, functional groups such as silicon groups and amino groups are connected to the surface of the modified glucan, so that the passing rates of various natural antioxidant components such as alpha-limonene, beta-caryophyllene, 1-phenanthrene, zingiberene, alpha-pinene, bergamotene, isorhamnetin, kaempferol humulene, gamma-terpinene, bisabolene, hyperoside, rutin and quercetin can be increased while anthraquinone is adsorbed, the loss of white in chromatography operation of the beneficial components is avoided, and the capacity of the polygonum flaccidum extract liquid for removing free radicals is enhanced. When the modified glucan prepared by the invention is used for preparing the polygonum flaccidum extraction liquid, the residual amount of anthraquinone can be effectively reduced, and the anthraquinone is harmful to human bodies and can also have adverse effects on strains used for distiller's yeast fermentation, such as slow growth and toxic substances generated by microorganisms in a stress state; therefore, when the modified glucan prepared by the invention is used for preparing the polygonum flaccidum extraction liquid, the distiller's yeast fermentation strain can obtain a better living environment, so that more fusel with unique flavor and derivative esters thereof are fermented, and the unique smell and flavor are provided for the finally prepared health-care rice wine. The health-care rice wine prepared by the invention contains abundant active ingredients such as flavonoids, terpenoids, amino acids and the like which can calm the nerves and nourish the heart, can relieve the emotion and relax the body and mind, and reduces the occurrence of insomnia.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of (0.5-1.5): 3-5): 62-68: (1-3), and stirring at a rotating speed of 300-500rpm at 38-42 ℃ for 4-6 hours to obtain an intermediate product;
m2, cutting the dialysis bag into 18-22cm, boiling the dialysis bag at 95-100 ℃ for 8-12min by using a sodium bicarbonate aqueous solution and an ethylene diamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the mass ratio of the dialysis bag to the sodium bicarbonate water solution to the ethylene diamine tetraacetic acid water solution is (0.8-1.4) to (2.7-3.3) to (2.9-4.1); the concentration of the aqueous sodium bicarbonate solution is 1.8-2.4wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 0.8-1.3mmol/L;
soaking the M3 in water at 18-22 deg.C for pretreatment of dialysis bag for 22-30min to obtain washed dialysis bag; the mass ratio of the pretreatment dialysis bag to the water is (0.8-1.3) to (4.5-6.5);
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 4-6d at 4-6 ℃, and then drying for 0.5-2h at 55-65 ℃ under the condition of vacuum degree of 0.08-0.2kPa to obtain the modified glucan.
The synergist is at least one of 6-amino nicotinic acid and bis (trimethylsilyl) carbodiimide; preferably, the synergist is a mixture of 6-aminonicotinic acid and bis (trimethylsilyl) carbodiimide according to a mass ratio of (1-4) to (1-3).
The invention has the beneficial effects that: the health-care rice wine disclosed by the invention is pleasant in flavor and unique in taste, and has good antioxidation and insomnia relieving effects.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
Introduction of some of the raw materials in this application:
glutinous rice, purchased from the food and oil company, the breed: fragrant glutinous rice, the water content is less than or equal to 10%, the polished rice rate is more than or equal to 61%, the impurity content is less than or equal to 1.0%, the product number is: 001.
cassava, purchased from fresh fruit source agriculture ltd, guangxiang county, variety: south China No. seven, integrity: 92 percent.
The rice is purchased from good agricultural products limited of fish platforms, the polished rice rate is 74 percent, the chalkiness rate is less than or equal to 15 percent, the chalkiness rate is less than or equal to 3 percent, and the protein content is as follows: 10%, the glue consistency is more than or equal to 65mm, and the amylose content: 20 percent.
Wheat, purchased in Zibo Zichuan province agricultural product professional cooperative, variety: selenium-rich small face, 1.0% of impurities, cargo number: 5464564.
gastrodia elata, tuckahoe, liquorice, dried orange peel and mulberry are purchased from Chengdu millet Shangpin pharmaceutical industry Co.
Pectinase, CAS:9032-75-1, food grade 30000U/g, from Biotechnology, inc., of Hebei Chuang origin.
Cellulase, CAS:9012-54-8, available from Beijing Solebao technologies, inc., food grade, 50000U/g.
Yeast: saccharomyces cerevisiae, CGMCC:2.3973, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
Koji mold: aspergillus japonicus, CGMCC:3.11440, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
Mucor circinelloides: mucor circinelloides, CGMCC:3.7107, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
Bacillus pumilus: bacillus pumilus, CGMCC:1.4441, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
The agrobacterium tumefaciens: glutamicibacter soli, CGMCC:1.8103, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
Lactobacillus plantarum: lactobacillus plantarum, CGMCC:1.12934, purchased from China general microbiological culture Collection center. The viable bacteria concentration is 10 7 CFU/g。
Glucose, CAS:50-99-7, available from western chemistry technologies (Shandong) Inc., product catalog number: a10187-500g.
Polygonum flaccidum: polygonum hydropiper L, purchased from Yihongtang pharmaceutical Co., ltd, bozhou, 1.5-3cm long and 1-2cm wide.
Hydrochloric acid, CAS:7647-01-0, available from Nanjing Chemicals GmbH, cat #: c1020210023, and the mass fraction is: 25 percent.
Absolute ethanol, CAS:64-17-5, available from Nanjing Chemicals, inc., cat #: C0692035010.
dextran, CAS:9004-54-0, available from chemical technology of west asia (Shandong) Inc., cat #: l14774-500g, molecular weight: 7 ten thousand.
Linoleic acid, CAS:60-33-3, available from western chemistry technologies (Shandong) Inc., cat #: a16095-500ml.
Dimethylsulfoxide, CAS:67-68-5, available from western chemical technology (Shandong) Inc., cat # s: a296671-500ml.
Aminonicotinic acid, CAS:3167-49-5, available from western chemical technology (Shandong) Inc., cat #: a13529-100g, purity more than or equal to 98.0%.
Bis (trimethylsilyl) carbodiimides, available from sahn chemical technology (shanghai) ltd, cat # no: 344338, purity: 98 percent.
Sodium bicarbonate, CAS:144-55-8, available from western chemical technology (Shandong) Inc., cat #: c10227-500g.
Ethylenediaminetetraacetic acid, CAS:60-00-4, available from western chemistry technologies (Shandong) Inc., cat #: c10227-500g.
Dialysis bags, available from beijing solibao technologies ltd, model: MD25, molecular weight 12000D, length 5m, crush width 25mm.
Example 1
A preparation method of health rice wine comprises the following steps:
a1, mixing sticky rice, cassava, rice, wheat and water according to a mass ratio of 1;
a2, cooling the fermentation material to 35 ℃, adding distiller's yeast and water, and fermenting for 65 hours to obtain crude wine; the mass ratio of the fermentation material to the distiller's yeast to the water is 5;
a3, filtering the crude wine to obtain a filtrate; sterilizing the filtrate at 65 deg.C with high-voltage pulse electric field to obtain health rice wine; the electric field intensity of the high-voltage pulse electric field is 50kV/cm, the pulse width is 400 mus, the pulse frequency is 10Hz, the pulse number is 10, and the processing time is 1s.
The distiller's yeast is prepared by the following method:
s1, mixing glutinous rice, cassava, rice and wheat according to a mass ratio of 1;
s2, mixing the dry powder and water according to a mass ratio of 1; then steaming and boiling for 45min at 100 ℃ to obtain cooked slurry;
s3, sterilizing the cooked slurry at 65 ℃ by using a high-voltage pulse electric field to obtain the sterilized cooked slurry; the electric field intensity of the high-voltage pulse electric field is 50kV/cm, the pulse width is 400 microseconds, the pulse frequency is 10Hz, the pulse number is 10, and the processing time is 1 second;
s4, concentrating the sterilized cooked slurry for 1 hour at 60 ℃ under the condition of vacuum degree of 35kPa, and then cooling to 35 ℃ to obtain concentrated slurry;
s5, inoculating a fermentation strain into the concentrated slurry, adding glucose and a polygonum hydropiper extract, and fermenting for 15d at the temperature of 35 ℃ and the relative humidity of 90% in an aseptic environment to obtain the distiller' S yeast; the mass ratio of the fermentation strain to the concentrated slurry to the glucose to the polygonum hydropiper extract is 5; the fermentation strain is a mixture of yeast, aspergillus japonicus, mucor circinelloides, bacillus pumilus, agrobacterium tumefaciens and lactobacillus plantarum in a mass ratio of 4.
The preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum thunb at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum thunb concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column;
h4, loading the polygonum flaccidum concentrated solution into a chromatographic column at 30 ℃, collecting filtrate, and concentrating the filtrate for 1H at 60 ℃ under the vacuum degree of 0.1kPa to obtain polygonum flaccidum extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of 1; the synergist is a mixture of 6-amino nicotinic acid and bis (trimethylsilyl) carbonyldiimine according to a mass ratio of 1;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylene diamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
soaking the pre-treatment dialysis bag for 25min by using water at the temperature of 20 ℃ by using M3 to obtain a dialysis bag after water washing; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the condition of 0.1kPa vacuum degree to obtain the modified glucan.
Example 2
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum thunb at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum thunb concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of 1; the synergist is 6-amino nicotinic acid;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylene diamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
m3, soaking the pretreatment dialysis bag with water at 20 ℃ for 25min to obtain a water-washed dialysis bag; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the vacuum degree of 0.1kPa to obtain the modified glucan.
Example 3
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of 1; the synergist is bis (trimethylsilyl) carbonyldiimine;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylene diamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
m3, soaking the pretreatment dialysis bag with water at 20 ℃ for 25min to obtain a water-washed dialysis bag; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the condition of 0.1kPa vacuum degree to obtain the modified glucan.
Comparative example 1
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum thunb at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum thunb concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid and dimethyl sulfoxide according to a mass ratio of 1;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylene diamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
soaking the pre-treatment dialysis bag for 25min by using water at the temperature of 20 ℃ by using M3 to obtain a dialysis bag after water washing; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the condition of 0.1kPa vacuum degree to obtain the modified glucan.
Comparative example 2
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum thunb at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum thunb concentrated solution;
soaking the glucan in the H2 hydrochloric acid-alcohol solution at 25 ℃ for 25 hours, and simultaneously performing ultrasonic treatment with the power of 380W and the frequency of 38kHz to obtain pretreated glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the glucan is 2.3;
h3, filling the pretreated glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading amount of the glucan in the chromatographic column is 75% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
Comparative example 3
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum concentrated solution;
h2, soaking polyamide in hydrochloric acid-alcohol solution at 25 ℃ for 25H, and simultaneously performing ultrasonic treatment with power of 380W and frequency of 38kHz to obtain pretreated polyamide; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the polyamide is 2.3;
h3, filling the pretreated polyamide into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated polyamide; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading of the polyamide in the chromatographic column is 75% of the volume of the column;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
Comparative example 4
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum concentrated solution;
soaking the modified glucan in absolute ethyl alcohol at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the mass ratio of the absolute ethyl alcohol to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column;
h4, loading the polygonum flaccidum concentrated solution into a chromatographic column at 30 ℃, collecting filtrate, and concentrating the filtrate for 1H at 60 ℃ under the vacuum degree of 0.1kPa to obtain polygonum flaccidum extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of 1; the synergist is a mixture of 6-amino nicotinic acid and bis (trimethylsilyl) carbodiimide according to a mass ratio of 1;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylene diamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylenediamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
soaking the pre-treatment dialysis bag for 25min by using water at the temperature of 20 ℃ by using M3 to obtain a dialysis bag after water washing; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the condition of 0.1kPa vacuum degree to obtain the modified glucan.
Comparative example 5
As in example 1, the only difference is: the preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
drying herba Polygoni Hydropiperis at 45 deg.C for 1 hr, pulverizing, sieving with 50 mesh sieve, adding water, decocting at 90 deg.C for 45min, and concentrating at 60 deg.C under vacuum degree of 0.1kPa for 1 hr to obtain herba Polygoni Hydropiperis extractive solution.
Comparative example 6
As in example 1, the only difference is: the distiller's yeast is prepared by the following method:
s1, mixing glutinous rice, cassava, rice and wheat according to a mass ratio of 1;
s2, mixing the dry powder and water according to a mass ratio of 1; then steaming and boiling for 45min at 100 ℃ to obtain cooked slurry;
s3, sterilizing the cooked slurry at 65 ℃ by using a high-voltage pulse electric field to obtain sterilized cooked slurry; the electric field intensity of the high-voltage pulse electric field is 50kV/cm, the pulse width is 400 microseconds, the pulse frequency is 10Hz, the pulse number is 10, and the processing time is 1 second;
s4, concentrating the sterilized cooked slurry for 1 hour at 60 ℃ under the condition of vacuum degree of 35kPa, and then cooling to 35 ℃ to obtain concentrated slurry;
s5, inoculating a fermentation strain into the concentrated slurry, adding glucose, and fermenting for 15d at 35 ℃ and at a relative humidity of 90% in an aseptic environment to obtain the distiller' S yeast; the mass ratio of the fermentation strain to the concentrated slurry to the glucose is 5; the fermentation strain is a mixture of yeast, aspergillus japonicus, mucor circinelloides, bacillus pumilus, agrobacterium tumefaciens and lactobacillus plantarum in a mass ratio of 4.
Example 4
A preparation method of health rice wine comprises the following steps:
a1, mixing sticky rice, cassava, rice, wheat and water according to a mass ratio of 1;
a2, cooling the fermentation material to 35 ℃, uniformly mixing the fermentation material with the composite nutrient material, adding distiller's yeast and water, and fermenting for 65 hours to obtain crude wine; the mass ratio of the fermentation material to the distiller's yeast to the water is 5; the mass ratio of the composite nutrient material to the fermentation material is 1;
a3, filtering the crude wine to obtain a filtrate; sterilizing the filtrate at 65 deg.C with high-voltage pulse electric field to obtain health rice wine; the electric field intensity of the high-voltage pulse electric field is 50kV/cm, the pulse width is 400 mus, the pulse frequency is 10Hz, the pulse number is 10, and the processing time is 1s.
The preparation method of the composite nutrient material comprises the following steps: washing rhizoma gastrodiae, poria cocos, liquorice, dried orange peel and mulberry with water, airing, and crushing to 100 meshes to obtain mixed powder, wherein the mass ratio of the rhizoma gastrodiae to the poria cocos to the liquorice to the dried orange peel to the mulberry is 0.5; mixing the mixed powder with water according to a mass ratio of 1; after the enzymolysis is finished, heating to 100 ℃ and keeping for 5min; cooling to room temperature, performing ultrasonic treatment at 300W and 25kHz for 20min, centrifuging, and collecting supernatant.
The distiller's yeast is prepared by the following method:
s1, mixing sticky rice, cassava, rice and wheat according to a mass ratio of 1;
s2, mixing the dry powder and water according to a mass ratio of 1; then steaming and boiling for 45min at 100 ℃ to obtain cooked slurry;
s3, sterilizing the cooked slurry at 65 ℃ by using a high-voltage pulse electric field to obtain the sterilized cooked slurry; the electric field intensity of the high-voltage pulse electric field is 50kV/cm, the pulse width is 400 microseconds, the pulse frequency is 10Hz, the pulse number is 10, and the processing time is 1 microsecond;
s4, concentrating the sterilized cooked slurry for 1 hour at 60 ℃ under the condition of vacuum degree of 35kPa, and then cooling to 35 ℃ to obtain concentrated slurry;
s5, inoculating a fermentation strain into the concentrated slurry, adding glucose and a polygonum flaccidum extraction liquid, and fermenting for 15d at 35 ℃ and a relative humidity of 90% in an aseptic environment to obtain the distiller' S yeast; the mass ratio of the fermentation strain, the concentrated slurry, the glucose and the polygonum hydropiper extraction liquid is (5); the fermentation strain is a mixture of saccharomycetes, aspergillus japonicus, mucor circinelloides, bacillus pumilus, agrobacterium tumefaciens and lactobacillus plantarum in a mass ratio of (4).
The preparation method of the polygonum flaccidum extraction liquid comprises the following steps:
h1, drying polygonum flaccidum at 45 ℃ for 1H, crushing, sieving with a 50-mesh sieve, adding water, decocting at 90 ℃ for 45min, and concentrating at 60 ℃ under the vacuum degree of 0.1kPa for 1H to obtain polygonum flaccidum concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 25 ℃ for 25 hours by using H2, and treating by using ultrasonic waves with power of 380W and frequency of 38kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 1mol/L, and the concentration of ethanol is 55wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is 2.3;
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 200cm, and the diameter of the chromatographic column is 18cm; the loading capacity of the modified glucan in the chromatographic column is 75% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, collecting filtrate at the chromatographic flow rate of 180mL/H, and concentrating the filtrate for 1H at the temperature of 60 ℃ and the vacuum degree of 0.1kPa to obtain polygonum hydropiper extract.
The preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of 1; the synergist is a mixture of 6-amino nicotinic acid and bis (trimethylsilyl) carbonyldiimine according to a mass ratio of 1;
m2, cutting the dialysis bag into 20cm, boiling the dialysis bag at 100 ℃ for 10min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate aqueous solution and the ethylene diamine tetraacetic acid aqueous solution are in a mass ratio of 1; the concentration of the aqueous sodium bicarbonate solution was 2wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 1mmol/L;
m3, soaking the pretreatment dialysis bag with water at 20 ℃ for 25min to obtain a water-washed dialysis bag; the mass ratio of the pretreatment dialysis bag to water is 1;
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 5d at 5 ℃, and then drying for 1h at 60 ℃ under the condition of 0.1kPa vacuum degree to obtain the modified glucan. The flavor test of example 4 was conducted by referring to the method of test example 3, and the odor was 9.86 points and the taste was 9.83 points.
Test example 1
Testing the residual quantity of anthraquinone: respectively putting 2g of the polygonum hydropiper extract obtained in the examples and the comparative examples into a 50mL centrifuge tube, adding 0.5mL anthraquinone-D8, adding 20mL n-hexane-acetone, homogenizing at 10000rpm for 0.5min, adding 0.2g of sodium chloride, performing vortex treatment for 1min, centrifuging at 4000rpm for 3min, transferring the upper layer extract solution into a concentration bottle, cleaning the head of the homogenizer with 20mL n-hexane-acetone, pouring the extract into residues, performing vortex treatment for 1min, performing centrifugal treatment at 4000rpm for 3min, combining the extracts, and concentrating to constant weight at 40 ℃ under the condition of 1 kPa. Then dissolving the residue with 3mL of n-hexane, transferring to a purification column, adding 50mL of n-hexane-ether mixed solvent at a flow rate of 3mL/min, collecting all eluates, concentrating at 40 deg.C under a pressure of 1kPa to constant weight, adding 2.0mL of acetone to dissolve the residue, mixing, filtering with 0.22 μm filter membrane, and determining with gas chromatography-mass spectrometry/mass spectrometry.
Gas chromatography-mass spectrometry/mass spectrometry conditions: the chromatographic column is HP-5MS with the size specification of 30m multiplied by 0.25mm multiplied by 0.25 mu m; the column temperature is programmed to be 100 ℃ and kept for 1min, and the temperature is increased to 300 ℃ at the speed of 20 ℃/m and kept for 10min; the carrier gas is helium with the purity of 99.999 percent, and the flow rate is 1.0mL/min; the temperature of a sample inlet is 300 ℃; the sample injection mode is non-shunting sample injection, and the valve is opened after 1 min; the sample injection amount is 1 mu L; the ionization mode is EI; the ionization energy is 70eV; the ion source temperature is 280 ℃; the interface temperature is 300 ℃; the determination mode is a reaction monitoring mode (SRM); the ion pairs were monitored as anthraquinone and anthraquinone-D8.
Calculating the residual amount of anthraquinone in the sample by using a chromatographic data processor according to the following formula: x = (c × V × 1000)/(m × 1000), where X is the residual amount of anthraquinone in the sample, in mg/kg; c is the concentration of anthraquinone solution obtained from the standard curve, and the unit is mug/mL; v is the final constant volume of the sample liquid, and the unit is mL; m is the mass of the sample represented by the final sample solution, and is given in g. The test results are shown in table 1.
TABLE 1 residual anthraquinone in Polygonum hydropiper extract
The residual amount of anthraquinone in example 1 was lower than in examples 2 to 3 and comparative examples 1 to 5. The possible reasons are: the 6-amino nicotinic acid contains carboxyl and amino with stronger polarity, and the two groups have specific relative positions so as to have a specific electronegativity center; the relative position and spatial configuration of carbonyl and silicon in bis (trimethylsilyl) carbonyldiimine enable the bis (trimethylsilyl) carbonyldiimine to have polarity within a specific range, the combination of the two is used as a synergist to promote the long-chain structure of linoleic acid to be cross-linked with glucan molecules in a spiral winding manner, the spatial entanglement complexity of glucan is further improved, the number ratio of introduced carboxyl, amino, carbonyl and silicon can form specific electronegativity strength, the adsorption effect on anthraquinone in polygonum hydropiper concentrated solution is enhanced, and the residual amount of anthraquinone in the prepared polygonum hydropiper extract is reduced.
Test example 2
DPPH free radical scavenging ability test: dissolving a DPPH reagent in absolute ethyl alcohol to obtain DPPH stock solution with the concentration of 2 mmol/L; respectively preparing the polygonum flaccidum extraction liquid obtained in the embodiment and the comparative example with water according to the mass ratio of 1; sequentially taking 7 kinds of samples with gradient concentration of 2mL each, adding 2.0mL of the stock solution of LDPPH, reacting at room temperature in the dark for 30min, shaking up, measuring the light absorption value, and recording the light absorption value at 517nm as A j (ii) a 2mL of pure water was added to each of the 7 samples at each gradient concentration of 2mL, and the absorbance at 517nm was recorded as A i . The control group is 2mL of DPPH solution added with 2mL of pure water, and the light absorption value is recorded as A c . The DPPH radical clearance, DPPH radical clearance (%) = (A) was calculated by the following formula i －A j )/A c X100%. The test results are shown in table 2.
TABLE 2 Eleocharis flabellifolia extract liquor for eliminating DPPH free radical
The DPPH free radical clearance rate of the embodiment 1 is higher than that of the embodiments 2-3 and the comparative examples 1-4, because the modified glucan prepared by the invention can increase the passing rate of various natural antioxidant components such as alpha-limonene, beta-caryophyllene, 1-phenanthrene, zingiberene, alpha-pinene, bergamotene, isorhamnetin, kaempferol humulene, gamma-terpinene, bisabolene, hyperoside, rutin and quercetin while adsorbing anthraquinone due to the fact that functional groups such as silicon groups and amino groups are grafted on the surface of the modified glucan when the modified glucan is used for chromatography of the polygonum hydropiper concentrated solution, the white loss of the beneficial components in chromatography operation is avoided, and the capacity of the finally obtained polygonum hydropiper extract for scavenging free radicals is enhanced.
Test example 3
Flavor testing: selecting 60 adults of 18-28 years old (50% of both men and women) with normal smell and taste as subjects; each subject tasted 2mL each time, and rinsed with 37 deg.C distilled water for 5min before and after each taste; each testee scores the smell and taste of the health rice wine obtained in the examples and the comparative examples, and each index is fully divided into 10 points; the evaluation criteria of the odor are pleasant aroma (8-10 points), moderate aroma (4-7 points) and bad odor (0-3 points); the evaluation standard of the taste is delicious (8-10 points), generally (4-7 points) and bad (0-3 points); the scores of the two indexes obtained in each example and comparative example are obtained by adding the scores of the two 60 subjects respectively and dividing the sum by 60. The test results are shown in table 3.
TABLE 3 flavor scores for health rice wine
The odor score and the taste score of example 1 are obviously better than those of examples 2-3 and comparative examples 1-6, because the modified glucan prepared by the invention can effectively reduce the residual amount of anthraquinone when being used for preparing the polygonum flaccidum extract, and anthraquinone is harmful to human bodies and can also have adverse effects on strains used for distiller's yeast fermentation, such as slow growth and toxic substances generated by microorganisms under a stress state; therefore, when the modified glucan prepared by the invention is used for preparing the polygonum flaccidum extraction liquid, the distiller's yeast fermentation strain can obtain a better living environment, so that more fusel with unique flavor and derivative esters thereof are fermented, and the unique smell and flavor are provided for the finally prepared health-care rice wine.
Test example 4
And (3) testing the insomnia relieving capacity: 160 subjects suffering from long-term insomnia, with the ages of 25-45 years and half of men and women are selected and divided into 4 groups of 40 persons, wherein one group serves as a control group; the control group did not eat the health rice wine obtained in examples 1-3 of the present invention and used 100mL of distilled water as a blank control, after drinking 100mL of the health rice wine 1h before sleeping every day; the test period is 28 days, the number of insomnia people per day in the test period is counted, the insomnia relieving capacity is measured by the sleeping time of each night, and the longer the sleeping time is, the more serious the insomnia is. The time to sleep of each subject was averaged over each group as the time to sleep data for that group. The test results are shown in table 4.
TABLE 4 health Rice wine for relieving insomnia
The time to sleep for examples 1-3 was significantly less than the time to sleep for the reference group. The health-care rice wine contains abundant active ingredients such as flavonoids, terpenes and amino acids which can calm the nerves and nourish the heart, can relieve the emotion and relax the body and mind, and reduces the occurrence of insomnia.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the present invention.
Claims (8)
1. A preparation method of health-care rice wine is characterized by comprising the following steps:
a1, mixing sticky rice, cassava, rice, wheat and water according to a mass ratio of (0.5-1.5): (0.5-1.3): (0.4-1.6): 0.2-1.5): 5.5-10), and cooking at 95-100 ℃ for 45-70min to obtain a fermented material;
a2, cooling the fermentation material to 33-36 ℃, uniformly mixing the fermentation material with the composite nutrient material, adding distiller's yeast and water, and fermenting for 63-75 hours to obtain crude wine; the mass ratio of the fermentation material to the distiller's yeast to the water is (3.5-5.5) to (0.5-1.5) to (10-20); the mass ratio of the composite nutrient material to the fermentation material is 1 (8-12);
a3, filtering the crude wine to obtain a filtrate; sterilizing the filtrate at 63-67 deg.C with high-voltage pulse electric field to obtain health rice wine.
2. The method for preparing rice wine for health protection as claimed in claim 1, wherein: the preparation method of the composite nutrient material comprises the following steps: washing rhizoma gastrodiae, poria cocos, liquorice, dried orange peel and mulberry with water, drying in the air, and crushing to 50-100 meshes to obtain mixed powder, wherein the mass ratio of the rhizoma gastrodiae to the poria cocos to the liquorice to the dried orange peel to the mulberry is (0.2-0.6) to (1-2); mixing the mixed powder with water according to the mass ratio of 1 (10-15), adding a complex enzyme, performing enzymolysis for 50-60min at 40-60 ℃ and 50-100rpm, wherein the mass ratio of the complex enzyme to the mixed powder is (1-5) to 100, and the complex enzyme is formed by mixing pectinase and cellulase according to the mass ratio of 1 (1-3); after the enzymolysis is finished, heating to 95-100 ℃ and keeping for 3-5min; cooling to room temperature, performing ultrasonic treatment at 20-30kHz and 200-350W for 10-30min, centrifuging, and collecting supernatant.
3. The method for preparing rice wine for health care according to claim 1, wherein the koji is prepared by the following method:
s1, mixing glutinous rice, cassava, rice and wheat according to a mass ratio of (1-5) to (1-5), drying at 45-55 ℃ for 0.5-2h, and then crushing and sieving with a 20-40-mesh sieve to obtain dry powder;
s2, mixing the dry powder and water according to a mass ratio of (0.7-1.3) to (2.5-4.2), stirring at a rotating speed of 25-35rpm for 2-4h at 22-27 ℃, and simultaneously carrying out ultrasonic treatment with power of 320-350W and frequency of 38-42 kHz; then steaming and boiling for 40-48min at 90-110 ℃ to obtain cooked slurry;
s3, sterilizing the cooked slurry at 62-68 ℃ by using a high-voltage pulse electric field to obtain sterilized cooked slurry; the electric field intensity of the high-voltage pulse electric field is 48-52kV/cm, the pulse width is 380-420 mus, the pulse frequency is 8-12Hz, the pulse number is 4-24, and the processing time is 0.5-2s;
s4, concentrating the sterilized cooked slurry for 0.8-2h at 58-62 ℃ under the vacuum degree of 33-38kPa, and then cooling to 33-38 ℃ to obtain concentrated slurry;
s5, inoculating a fermentation strain into the concentrated slurry, adding glucose and polygonum hydropiper extract, and fermenting for 14-20 days at the temperature of 33-38 ℃ and the relative humidity of 80-92% in an aseptic environment to obtain the distiller' S yeast; the mass ratio of the fermentation strain, the concentrated slurry, the glucose and the polygonum hydropiper extract is (3-7): 90-115): 20-25): 4-7; the fermentation strain is a mixture of microzyme, aspergillus japonicus, mucor circinelloides, bacillus pumilus, soil glutamic acid bacillus and lactobacillus plantarum according to the mass ratio of (1-6) to (1-6).
4. The preparation method of the health rice wine as claimed in claim 3, wherein the preparation method of the polygonum flaccidum extract comprises the following steps:
h1, drying polygonum flaccidum herb at 42-48 ℃ for 0.5-2H, crushing, sieving with a 40-60-mesh sieve, adding water, decocting at 85-92 ℃ for 40-48min, and concentrating at 55-62 ℃ under the vacuum degree of 0.08-0.3kPa for 0.5-1.5H to obtain polygonum flaccidum herb concentrated solution;
soaking the modified glucan in hydrochloric acid-alcohol solution at 23-27 ℃ for 24-30H by using H2, and treating by using ultrasonic waves with power of 360-400W and frequency of 36-40kHz to obtain pretreated modified glucan; the concentration of chloride ions in the hydrochloric acid-alcohol solution is 0.8-1.2mol/L, and the concentration of ethanol is 50-58wt.%; the mass ratio of the hydrochloric acid-alcohol solution to the modified glucan is (1.8-3.2) to (0.7-1.3);
h3, filling the pretreated modified glucan into a chromatographic column, and then adding absolute ethyl alcohol into the chromatographic column until the absolute ethyl alcohol just submerges the pretreated modified glucan; the length of the chromatographic column is 190-210cm, and the diameter is 16-19cm; the loading capacity of the modified glucan in the chromatographic column is 70-80% of the volume of the column body;
h4, loading the polygonum hydropiper concentrated solution into a chromatographic column at the temperature of 30 ℃, wherein the chromatographic flow rate is 170-190mL/H, collecting filtrate, and concentrating the filtrate for 1H at the temperature of 55-65 ℃ and the vacuum degree of 0.08-0.2kPa to obtain polygonum hydropiper extract.
5. The method for preparing rice wine for health protection as claimed in claim 4, wherein: the preparation method of the modified glucan comprises the following steps:
m1, mixing glucan, linoleic acid, dimethyl sulfoxide and a synergist according to a mass ratio of (0.5-1.5): 3-5): 62-68: (1-3), and stirring at a rotating speed of 300-500rpm at 38-42 ℃ for 4-6 hours to obtain an intermediate product;
m2, cutting the dialysis bag into 18-22cm, boiling the dialysis bag at 95-100 ℃ for 8-12min by using a sodium bicarbonate aqueous solution and an ethylenediamine tetraacetic acid aqueous solution, cooling to room temperature, and draining to obtain a pretreatment dialysis bag; the dialysis bag, the sodium bicarbonate water solution and the ethylene diamine tetraacetic acid water solution have the mass ratio of (0.8-1.4) to (2.7-3.3) to (2.9-4.1); the concentration of the aqueous sodium bicarbonate solution is 1.8-2.4wt.%; the concentration of the ethylene diamine tetraacetic acid aqueous solution is 0.8-1.3mmol/L;
soaking the M3 in water at 18-22 deg.C for pretreatment of dialysis bag for 22-30min to obtain washed dialysis bag; the mass ratio of the pretreatment dialysis bag to the water is (0.8-1.3) to (4.5-6.5);
m4, putting the intermediate product obtained in the step M1 into a dialysis bag after water washing, dialyzing for 4-6d at 4-6 ℃, and then drying for 0.5-2h at 55-65 ℃ under the condition of vacuum degree of 0.08-0.2kPa to obtain the modified glucan.
6. The method for preparing rice wine for health protection as claimed in claim 5, wherein: the synergist is at least one of 6-amino nicotinic acid and bis (trimethylsilyl) carbodiimide.
7. The method for preparing rice wine for health protection as claimed in claim 1, wherein: the electric field intensity of the high-voltage pulse electric field is 48-52kV/cm, the pulse width is 380-430 mus, the pulse frequency is 8-12Hz, the pulse number is 4-24, and the processing time is 0.5-2s.
8. A health rice wine is characterized in that: prepared by the method of any one of claims 1 to 7.
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