CN102994350B - Preparation method of tartary buckwheat wine with function of reducing blood fat - Google Patents
Preparation method of tartary buckwheat wine with function of reducing blood fat Download PDFInfo
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Abstract
The invention relates to a preparation method of a healthy wine, and in particular relates to a preparation method of a tartary buckwheat wine with a function of reducing blood fat. The preparation method comprises the following steps of: 1, extracting a tartary buckwheat extracting solution; 2, carrying out vacuum concentration on the tartary buckwheat extracting solution; 3, separating the concentrated solution by an activated resin column; 4, top-washing the resin column by using pure water until effluent becomes clear from muddy; 5, eluting the resin column by using 40-65% alcohol, detecting an eluent by using an ammonia water development process, when test paper becomes yellow from colorless and then changes into colorless, stopping eluting, and collecting the eluent; 6, carrying out vacuum concentration on the eluent for recovering alcohol, vacuum-drying to obtain a dry extract with the flavonoid content of 40-85 percent; and 7, selecting white wine with an alcoholic strength of 25-68%vol, adding the dry extract, fully uniformly stirring, standing for 24-48h, and filtering to obtain the tartary buckwheat wine. The tartary buckwheat wine prepared by adopting the preparation method has the flavonoid content being not less than 100mg/L, is safe and nontoxic, and has the effect of assisting the reduction of the blood fat.
Description
Technical field
The present invention relates to a kind of preparation method of health promoting wine, specifically a kind of preparation method with hypolipemic function Radix Et Rhizoma Fagopyri Tatarici wine.
Background technology
Radix Et Rhizoma Fagopyri Tatarici is a kind of Traditional Agricultural crop of China, plants with a long history.Belong to the polygonaceae dicotyledons, " Tuber Fleeceflower Root, the rheum officinale " that polygonaceae and people were familiar with etc. is blood brother.Compendium of Material Medica record: the Radix Et Rhizoma Fagopyri Tatarici nature and flavor are bitter, flat, cold, " real stomach, beneficial strength, continuous spirit, sharp knowledge, can practice the five internal organs dregs dirty ", " the wide intestines of sending down abnormally ascending, mill is stagnant, and the heat that disappears swells wind bitterly.Prescriptions Worth Thousand Gold for Emergencies, " florilegium paddy spectrum ", Important Arts for the People's Welfare etc. have saying that Radix Et Rhizoma Fagopyri Tatarici cures the disease.Radix Et Rhizoma Fagopyri Tatarici formal name used at school hull buckwheat, it is the outstanding grain medicine dual-purpose grain kind that international food and agricultural organization generally acknowledges, because Radix Et Rhizoma Fagopyri Tatarici contains Flavonoid substances, its major ingredient is rutin, current clinical medicine is observed and is shown, the Radix Et Rhizoma Fagopyri Tatarici mask has hypoglycemic, reducing blood-fat, strengthens body immunity, treatment stomach disease, removing dampness and detoxicating, controls the effect of disliking meat in ephritis, erosion body, and diabetes, hypertension, hyperlipidemia, coronary heart disease, apoplexy, patients with gastric disease are had to auxiliary therapeutic action.Also contain some trace elements K, magnesium and amino acids simultaneously, human body is had to good nourishing function.
Through retrieval, the method for preparing at present Radix Et Rhizoma Fagopyri Tatarici wine, as Chinese invention patent application 01107297.0,200810047249.2,200810047251.X etc., be all by Radix Et Rhizoma Fagopyri Tatarici by fermentation, the operation such as distillation is prepared from, and Radix Et Rhizoma Fagopyri Tatarici wine prepared by fermentation method, due to by fermentation, distillation process, its main composition overwhelming majority is lost, thereby adopts the white wine that Radix Et Rhizoma Fagopyri Tatarici is brewageed to have hardly hypolipemic function.Simultaneously, because the Radix Et Rhizoma Fagopyri Tatarici starch content is low, cause liquor output rate to only have 30%, far below the yield of liquor of Chinese sorghum 55%, it is almost 2 times of sorghum-brewed wine cost that the wine body is brewageed cost, and mouthfeel is poor, and human consumer's acceptance is not high.Following table is the detected result of the Radix Et Rhizoma Fagopyri Tatarici wine for preparing of fermentation method:
Summary of the invention
Purpose of the present invention just is to provide a kind of preparation method with hypolipemic function Radix Et Rhizoma Fagopyri Tatarici wine; The Radix Et Rhizoma Fagopyri Tatarici wine that the inventive method is prepared, wine and women-sensual pursuits is bright orange, and the wine body is soft, sweet tasty and refreshing, and aroma, Mai Xiang have both at the same time; Wherein flavones content is not less than 100mg/L, learn inspection center through Tongji Medical College, Huazhong Science and Technology Univ.'s function of health food and carry out acute toxicity test and animal reducing blood-fat test, result shows: the Radix Et Rhizoma Fagopyri Tatarici wine that the inventive method is prepared, safety non-toxic, have auxiliary lipid-lowering efficacy.
The inventive method comprises the steps:
1. extract: add its weight 12-20 ethanol of 50～80% doubly in Radix Et Rhizoma Fagopyri Tatarici, 70～90 ℃ of lower refluxing extraction 2-4 time, 1.5-3 hour at every turn; Merge extracting solution each, filter, obtain filtrate; Because mainly contain the compositions such as flavones, VITAMIN, amino acid, crude protein in Radix Et Rhizoma Fagopyri Tatarici, wherein Flavonoid substances is dissolved in ethanol, so at first take the extraction using alcohol Flavonoid substances.
2. concentrating under reduced pressure: filtrate is evaporated under 60～85 ℃ to every 1ml concentrated solution and is equivalent to Radix Et Rhizoma Fagopyri Tatarici 1g, obtain concentrated solution.
3. resin column separates: by the AB-8 resin column that on concentrated solution, overactivation is processed, upper prop speed is 3～6BV/H; When summation that collected effluent liquid is upper prop liquid and resin column volume, stop upper prop, static absorption 1-2 hour; Because the AB-8 resin has the characteristic of absorption flavones, after having carried out various contrast experiments, select the AB-8 resin to be separated extracting solution.
4. wash impurity elimination: wash resin column with the pure water top, elution speed is 4～6 BV/H, when effluent liquid becomes clarification from muddiness, stops washing; The water-soluble substances that is adsorbed on the AB-8 resin surface can be effectively removed in washing.
5. alcohol wash: the ethanol-eluting resin column with 40～65%, elution speed is controlled at 1～3 BV/H, with the ammoniacal liquor development process, detects elutriant, when test paper when becoming yellow and becoming colorless, stops wash-out from colourless, collects elutriant; The Flavonoid substances that ethanol with 40～65% can will be adsorbed on the AB-8 resin column elutes.
6. dry: the elutriant concentrating under reduced pressure is reclaimed to ethanol, and concentrated solution, in 70～90 ℃ of lower vacuum-dryings, obtains the dry extract that flavones content is 40～85%;
7. preparation: choose the white wine of alcoholic strength 25～68%vol, add the dry extract that above-mentioned flavones content is 40～85%, stir, standing 24-48 hour, filter, and obtains; Require flavones content in wine to be not less than 100mg/L
The Radix Et Rhizoma Fagopyri Tatarici wine that aforesaid method is prepared, wine and women-sensual pursuits is bright orange, and the wine body is soft, sweet tasty and refreshing, and aroma, Mai Xiang have both at the same time; Wherein flavones content is not less than 100mg/L.And the inventive method production cost is approximately 1/2nd of brewing wine.
Embodiment
Embodiment 1:
1. extract: add the ethanol of 600L 75% in 40kg Radix Et Rhizoma Fagopyri Tatarici (tartary buckwheat flavone content 2.7%), 70 ℃ of lower refluxing extraction 3 times, each 3 hours; Merge extracting solution each, filter, obtain filtrate;
2. concentrating under reduced pressure: filtrate is evaporated under 60 ℃ to every 1ml concentrated solution and is equivalent to Radix Et Rhizoma Fagopyri Tatarici 1g, obtain concentrated solution, detecting flavones content in concentrated solution is 1.1%, and tartary buckwheat flavone extracts the rate of transform 40.74%;
3. resin column activation: take the AB-8 resin, use successively resin demand 2-3 8% hydrochloric acid, pure water, 8%NaOH, pure water, 95% ethanol, pure water wash-out resin doubly, take the elutriant clarification as the wash-out terminal at every turn;
4. resin isolation: get on concentrated solution the AB-8 resin of activation treatment, upper prop speed is 5BV/H; When summation that collected effluent liquid is upper prop liquid and resin column volume, stop upper prop, static absorption 1 hour;
5. washing: wash resin column with the pure water top, elution speed is 6 BV/H, when effluent liquid becomes clarification from muddiness, stops washing;
6. alcohol wash: the ethanol-eluting resin column with 60%, elution speed is 3 BV/H, with the ammoniacal liquor development process, detects (after test paper is wetting with effluent liquid, put ammoniacal liquor reagent bottleneck and observe color, as be yellow, need to continue wash-out, when colourless, stop wash-out), collect elutriant;
7. dry: the elutriant concentrating under reduced pressure is reclaimed to ethanol, and concentrated solution is in 70 ℃ of lower vacuum-dryings, the dry extract 410g that to obtain flavones content be 51.34%;
8. preparation: the aromatic Chinese spirit 100L that to choose alcoholic strength be 45%vol, add the dry extract 42g that above-mentioned flavones content is 51.34%, stir, standing 24 hours, filter, obtain.In wine, flavones content is 152.8mg/L after testing.
Below the detected result of the prepared 45%vol Luzhou-flavor Radix Et Rhizoma Fagopyri Tatarici wine of the embodiment of the present invention 1:
By the Radix Et Rhizoma Fagopyri Tatarici wine of embodiment 1 preparation, send Tongji Medical College, Huazhong Science and Technology Univ.'s function of health food to learn inspection center and detected, report content is as follows:
One, test item: food safety evaluation on toxicology
Detect title: Radix Et Rhizoma Fagopyri Tatarici wine
Amount detection: 2500ml
Detect lot number: 2010005
Test basis: " protective foods check and evaluation technique standard " (version in 2003)
Detected result and judging: Radix Et Rhizoma Fagopyri Tatarici wine human body recommended intake every day is 100ml, and by adult 60kg batheroom scale, recommending to take in dosage is 1.67ml/kg.bw.The acute toxicity tests shows, the mld (LD of Radix Et Rhizoma Fagopyri Tatarici wine to mouse
50)>200.0 ml/kg.bw, true border non-toxic substance.Salmonella reversion test, Micronuclei In The Mouse Bone Marrow test and sperm malformation test are all negative.In 30 days feeding studys of rat, give tested material by 25 times, 50 times, 100 times of the human body recommended intake (41.7,83.4,167.0ml/kg.bw), and set up Normal group and solvent control group, measurement result shows respectively to organize the indexs such as rat body weight growth, food utilization, dirty body ratio, hematology and serum biochemistry all in range of normal value, and each dosage group does not have significance with the corresponding group difference that contrasts; There is no to find the toxic pathology relevant with tested material in liver,kidney,spleen, stomach and intestine, ovary and testopathy inspection yet.According to " protective foods check and evaluation technique standard " (version in 2003), the judgement Radix Et Rhizoma Fagopyri Tatarici wine is checked by food safety toxicology.
Two, test item: auxiliary antilipemic (animal experiment)
Detect title: Radix Et Rhizoma Fagopyri Tatarici wine
Amount detection: 2500ml
Detect lot number: 2010005
Test basis: " protective foods check and evaluation technique standard " (version in 2003)
Detected result and judgement: Radix Et Rhizoma Fagopyri Tatarici wine, the adult recommends take in 100ml every day, is converted into 1.67 ml/kg.bw.The disorderly model of lipid metabolism in rats, by 5,10,30 multiple doses (i.e. 8.35,16.7,50.1 ml/kg.bw) the preventative tested material that gives of dividing into groups of adult's recommended amounts, is established high fat control group (high lipid food), solvent control group and Normal group (basal feed) simultaneously.Test-results shows: give tested material after 30 days, compare with high fat control group, 16.7 ml/kg.bw, 50.1 ml/kg.bw dosage group TC, TG level significantly descend, and 8.35 ml/kg.bw, 16.7 ml/kg.bw dosage group HDL-C levels significantly raise.
Judge: according to " protective foods detects and the evaluation technique standard " (version in 2003), judge that Radix Et Rhizoma Fagopyri Tatarici wine has auxiliary lipid-lowering function to animal.
Embodiment 2:
1. extract: add the ethanol of 600L 80% in 40kg Radix Et Rhizoma Fagopyri Tatarici (tartary buckwheat flavone content 2.7%), 75 ℃ of lower refluxing extraction 4 times, each 3 hours; Merge extracting solution each, filter, obtain filtrate;
2. concentrating under reduced pressure: filtrate is evaporated under 65 ℃ to every 1ml concentrated solution and is equivalent to Radix Et Rhizoma Fagopyri Tatarici 1g, obtain concentrated solution, detecting flavones content in concentrated solution is 1.2%, and tartary buckwheat flavone extracts the rate of transform 44.44%;
3. resin column activation: take the AB-8 resin, use successively resin demand 2-3 8% hydrochloric acid, pure water, 8%NaOH, pure water, 95% ethanol, pure water wash-out resin doubly, take the elutriant clarification as the wash-out terminal at every turn;
4. resin isolation: get on concentrated solution the AB-8 resin of activation treatment, upper prop speed is 6BV/H; When summation that collected effluent liquid is upper prop liquid and resin column volume, stop upper prop, static absorption 2 hours;
5. washing: wash resin column with the pure water top, elution speed is 6 BV/H, when effluent liquid becomes clarification from muddiness, stops washing;
6. alcohol wash: the ethanol-eluting resin column with 65%, elution speed is 3 BV/H, with the ammoniacal liquor development process, detects (after test paper is wetting with effluent liquid, the actual bottleneck of aobvious ammoniacal liquor is observed color, as is yellow, needs to continue wash-out, when colourless, stop wash-out), collect elutriant;
7. dry: the elutriant concentrating under reduced pressure is reclaimed to ethanol, and concentrated solution is in 80 ℃ of lower vacuum-dryings, the dry extract 398g that to obtain flavones content be 59.22%%;
8. preparation: choose the fen-flavor type white spirit 100L of alcoholic strength 50%vol, add the dry extract 41g that above-mentioned flavones content is 59.22%, stir, standing 36 hours, filter, must ask flavones content in wine is 168mg/L.
Embodiment 3:
1. extract: add the ethanol of 600L 75% in 40kg Radix Et Rhizoma Fagopyri Tatarici (tartary buckwheat flavone content 2.7%), 75 ℃ of lower refluxing extraction 4 times, each 2.5 hours; Merge extracting solution each, filter, obtain filtrate;
2. concentrating under reduced pressure: filtrate is evaporated under 70 ℃ to every 1ml concentrated solution and is equivalent to Radix Et Rhizoma Fagopyri Tatarici 1g, obtain concentrated solution, detecting flavones content in concentrated solution is 1.3%, and the tartary buckwheat flavone extraction yield is 48.15%;
3. resin column activation: take the AB-8 resin, use successively resin demand 2-3 8% hydrochloric acid, pure water, 8%NaOH, pure water, 95% ethanol, pure water wash-out resin doubly, take the elutriant clarification as the wash-out terminal at every turn;
4. resin isolation: get on concentrated solution the AB-8 resin of activation treatment, upper prop speed is 6BV/H; When summation that collected effluent liquid is upper prop liquid and resin column volume, stop upper prop, static absorption 2 hours;
5. washing: wash resin column with the pure water top, elution speed is 6 BV/H, when effluent liquid becomes clarification from muddiness, stops washing;
6. alcohol wash: the ethanol-eluting resin column with 65%, elution speed is 3BV/H, with the ammoniacal liquor development process, detects (after test paper is wetting with effluent liquid, the actual bottleneck of aobvious ammoniacal liquor is observed color, as is yellow, needs to continue wash-out, when colourless, stop wash-out), collect elutriant;
7. dry: the elutriant concentrating under reduced pressure is reclaimed to ethanol, and concentrated solution is in 90 ℃ of lower vacuum-dryings, the dry extract 405g that to obtain flavones content be 61.11%;
8. preparation: choose the Maotai-flavor liquor 100L of alcoholic strength 68%vol, add the dry extract 44g that above-mentioned flavones content is 61.11%, stir, standing 48 hours, filter, must ask flavones content in wine is 152mg/L.
Alcohol concn used in the present invention is volume fraction, and hydrochloric acid, NaOH strength of solution are massfraction.
Claims (1)
1. the preparation method with hypolipemic function Radix Et Rhizoma Fagopyri Tatarici wine is characterized in that comprising following processing step:
(1) extract: add the ethanol of 600L 75% in the Radix Et Rhizoma Fagopyri Tatarici of 40kg tartary buckwheat flavone content 2.7%, 70 ℃ of lower refluxing extraction 3 times, each 3 hours; Merge extracting solution each, filter, obtain filtrate;
(2) concentrating under reduced pressure: filtrate is evaporated under 60 ℃ to every 1ml concentrated solution and is equivalent to Radix Et Rhizoma Fagopyri Tatarici 1g, obtain concentrated solution, detecting flavones content in concentrated solution is 1.1%, and tartary buckwheat flavone extracts the rate of transform 40.74%;
(3) resin column activation: take the AB-8 resin, use successively resin demand 2-3 8% hydrochloric acid, pure water, 8%NaOH, pure water, 95% ethanol, pure water wash-out resin doubly, take the elutriant clarification as the wash-out terminal at every turn;
(4) resin isolation: get on concentrated solution the AB-8 resin of activation treatment, upper prop speed is 5BV/H; When summation that collected effluent liquid is upper prop liquid and resin column volume, stop upper prop, static absorption 1 hour;
(5) washing: wash resin column with the pure water top, elution speed is 6 BV/H, when effluent liquid becomes clarification from muddiness, stops washing;
(6) alcohol wash: the ethanol-eluting resin column with 60%, elution speed is 3 BV/H, with the ammoniacal liquor development process, detects, test paper is wetting with effluent liquid after, put ammoniacal liquor reagent bottleneck and observe color, as be yellow, need to continue wash-out, when colourless, stop wash-out, the collection elutriant;
(7) dry: the elutriant concentrating under reduced pressure is reclaimed to ethanol, and concentrated solution is in 70 ℃ of lower vacuum-dryings, the dry extract 410g that to obtain flavones content be 51.34%;
(8) preparation: the aromatic Chinese spirit 100L that to choose alcoholic strength be 45%vol, add the dry extract 42g that above-mentioned flavones content is 51.34%, stir, standing 24 hours, filter, obtain; In wine, flavones content is 152.8mg/L after testing.
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| JP6192167B2 (en) * | 2014-03-28 | 2017-09-06 | 国立大学法人信州大学 | Fermented food extract composition |
| CN104371891B (en) * | 2014-11-10 | 2016-02-17 | 江苏洋河酒厂股份有限公司 | A kind of preparation method avenging chrysanthemum bitter-buckwheat nutritive wine |
| CN106723023A (en) * | 2016-11-29 | 2017-05-31 | 内蒙古医科大学 | A kind of lipid-lowering health food and preparation method thereof |
| CN108913499A (en) * | 2018-08-09 | 2018-11-30 | 劲牌生物医药有限公司 | A kind of tartary buckwheat extract and preparation method thereof, application and health liquor |
| CN112011421A (en) * | 2020-09-14 | 2020-12-01 | 劲牌有限公司 | Three-spice compound tartary buckwheat wine and production method thereof |
| CN113880895A (en) * | 2021-04-13 | 2022-01-04 | 温州大学 | Application of rutin in preparation of medicine for treating colon injury induced by diabetes |
| CN116813459B (en) * | 2023-06-28 | 2024-05-31 | 河南中医药大学 | Extraction method and application of wild buckwheat rhizome terpenoid |
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| CN101085958A (en) * | 2007-06-22 | 2007-12-12 | 山西省农业科学院农产品综合利用研究所 | Tartary buckwheat oxidation resistance health care wine |
| CN102302560A (en) * | 2011-09-01 | 2012-01-04 | 西昌市元农农业开发有限公司 | Composition of lucid ganoderma extract and tartary buckwheat extract, as well as application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101085958A (en) * | 2007-06-22 | 2007-12-12 | 山西省农业科学院农产品综合利用研究所 | Tartary buckwheat oxidation resistance health care wine |
| CN102302560A (en) * | 2011-09-01 | 2012-01-04 | 西昌市元农农业开发有限公司 | Composition of lucid ganoderma extract and tartary buckwheat extract, as well as application thereof |
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