CN101338329B - Method for preparing garlicin from garlic - Google Patents
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- CN101338329B CN101338329B CN2008101396000A CN200810139600A CN101338329B CN 101338329 B CN101338329 B CN 101338329B CN 2008101396000 A CN2008101396000 A CN 2008101396000A CN 200810139600 A CN200810139600 A CN 200810139600A CN 101338329 B CN101338329 B CN 101338329B
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Abstract
The invention relates to a method for preparing allicin from garlic which consists of the following steps: after the garlic is peeled, cracking and pulping; enzymatic conversion; ultrasonic extraction; impurity removing; vacuum condensing; spraying and drying; the method is characterized in that: in step b, water and/or ethanol is used as a solvent; the concentration of the ethanol is 0 to 50 percent or 100 percent; the garlic pulp and the solvent with a weight ratio of 1: 2 to 1: 6 is inputted into a reaction kettle; the reaction temperature is 30 to 50 DEG C; the reaction time is 60 to 120min. The method of the invention has the beneficial effects of no residue of harmful matters, simple process and short period; besides, the used chemical reagent accords with the environment protection. As the enzymatic conversion and ultrasonic extraction technology in a low temperature, removing macromolecule matters with ultrafiltration, membrane condensing and the freezing drying technology of low temperature preparing during the full process are adopted, the obtaining rate and the activation of the allicin are greatly improved; no harmful solvents are used; the cost is low; the method of the invention is applicable for industrial production.
Description
(1) technical field
The present invention relates to effective plant component extracting process, particularly a kind of method that from garlic, prepares garlicin.
(2) background technology
Garlic is the bulb of Liliaceae allium garlic, and cultivation is all arranged all over the world.Modern medicine confirms, the broad-spectrum sterilization treatment function of garlic, mainly be garlicin in action.The special garlic odour of garlic is exactly from garlicin.China's garlic resource is abundant, and numerous in variety, fine quality, the total volume of exports accounts for the 4th in the world, and in recent years, external many enterprises added garlicin to healthcare products such as medicine, to the also increase day by day of demand of people's allicin.Produce garlicin at present both at home and abroad and mainly contain two approach: first adopts the high-load garlicin of synthetic, and second extracts the garlicin of low levels from natural fresh garlic.Because synthetic allicin has residual harmful substance, can only be as the additive on the fodder industry.If must extract the garlicin of low levels as the additive of Medicines and Health Product from natural bright garlic, but the production technique of garlicin exists flow process complexity, cycle long now, problems such as the not environmental protection of chemical reagent of use.In sum, be necessary traditional garlicin extraction process is improved.
(3) summary of the invention
The present invention is in order to remedy the deficiencies in the prior art, provides a kind of unharmful substance is residual, flow process is simple, the cycle is short, use chemical reagent to meet the method for preparing garlicin from garlic of environmental protection.
The present invention is achieved through the following technical solutions:
The method for preparing garlicin from garlic of the present invention is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin;
C. ultrasonic extraction;
D. removal of impurities: after centrifugal solid-liquid separation, the secondary filter, carry out ultrafiltration, adopt ultra-filtration membrane to separate and removes macromolecular substance;
E. vacuum concentration: the clear liquid that obtains after the removal of impurities adopts the reverse osmosis concentration unit to carry out membrane concentration;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%;
Its special character is: among the step b, as solvent, its concentration is 0-100% with the alcoholic acid aqueous solution, and the garlic slurry is imported in the reactor than 1:2-6 with weight of solvent, temperature of reaction 30-50 ℃, and reaction times 60-120min.
The method for preparing garlicin from garlic of the present invention among the step c, will add above-mentioned solvent again in the material after the enzymatic conversion method, make the garlic slurry be transferred to 1:6-10 with the weight of solvent ratio, input ultrasonic extraction unit, ultrasonic frequency 25KHz handles 30-60min at normal temperature.
The method for preparing garlicin from garlic of the present invention, in the steps d, ultra-filtration membrane is mineral membrane or ceramic membrane, the ultra-filtration membrane molecular weight 8000-50000Da that dams.
The method for preparing garlicin from garlic of the present invention among the step e, concentrates at normal temperatures, is concentrated into solid content and reaches 25-35%.
The invention has the beneficial effects as follows that unharmful substance is residual, flow process is simple, and the cycle is short, and the chemical reagent of use meets environmental protection.Owing to adopt enzymatic conversion method, ultrasonic low temperature extractive technique, macromolecular substance is removed in ultrafiltration, membrane concentration and lyophilize whole process low-temperature fabrication, garlicin pick-up rate and activity have been improved greatly, the garlicin pick-up rate brings up to 95% from 30% of traditional technology, no hazardous solvent uses, and cost is low, is fit to suitability for industrialized production.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Accompanying drawing is a schematic flow sheet of the present invention.
(5) embodiment
Embodiment 1
The method for preparing garlicin from garlic of the present invention is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin, and solvent is the alcoholic acid aqueous solution, and its concentration is 25%, and garlic slurry and weight of solvent be than in the 1:5 input reactor, 45 ℃ of insulation 100min;
C. ultrasonic extraction: the material after the enzymatic conversion method adds above-mentioned solvent again, makes the garlic slurry be transferred to 1:8 with the weight of solvent ratio, input ultrasonic extraction unit, and ultrasonic frequency 25KHz handles 30min at normal temperature;
D. removal of impurities: centrifugal solid-liquid separates, after the secondary filter, carry out ultrafiltration, adopts ultra-filtration membrane to separate and removes macromolecular substance, and ultra-filtration membrane is a mineral membrane, the ultra-filtration membrane molecular weight 10000Da that dams;
E. vacuum concentration: separate clear liquid and adopt the reverse osmosis concentration unit, membrane concentration makes solid content reach 30% at normal temperatures;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%.
Embodiment 2
The method for preparing garlicin from garlic of the present invention is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin, and solvent is a water, and garlic slurry and weight of solvent be than in the 1:2 input reactor, 30 ℃ of insulation 120min;
C. ultrasonic extraction: the material after the enzymatic conversion method adds above-mentioned solvent again, makes the garlic slurry be transferred to 1:6 with the weight of solvent ratio, input ultrasonic extraction unit, and ultrasonic frequency 25KHz handles 60min at normal temperature;
D. removal of impurities: centrifugal solid-liquid separates, after the secondary filter, carry out ultrafiltration, adopts ultra-filtration membrane to separate and removes macromolecular substance, and ultra-filtration membrane is a mineral membrane, the ultra-filtration membrane molecular weight 8000Da that dams;
E. vacuum concentration: separate clear liquid and adopt the reverse osmosis concentration unit, membrane concentration makes solid content reach 25% at normal temperatures;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%.
Embodiment 3
The method for preparing garlicin from garlic of the present invention is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin, and solvent is the alcoholic acid aqueous solution, and its concentration is 50%, and garlic slurry and weight of solvent be than in the 1:6 input reactor, 50 ℃ of insulation 60min;
C. ultrasonic extraction: the material after the enzymatic conversion method adds above-mentioned solvent again, makes the garlic slurry be transferred to 1:10 with the weight of solvent ratio, input ultrasonic extraction unit, and ultrasonic frequency 25KHz handles 45min at normal temperature;
D. removal of impurities: centrifugal solid-liquid separates, after the secondary filter, carry out ultrafiltration, adopts ultra-filtration membrane to separate and removes macromolecular substance, and ultra-filtration membrane is a ceramic membrane, the ultra-filtration membrane molecular weight 50000Da that dams;
E. vacuum concentration: separate clear liquid and adopt the reverse osmosis concentration unit, membrane concentration makes solid content reach 35% at normal temperatures;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%.
Embodiment 4
The method for preparing garlicin from garlic of the present invention is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin, and solvent is the ethanol of concentration 100%, and garlic slurry and weight of solvent be than in the 1:4 input reactor, 40 ℃ of insulation 80min;
C. ultrasonic extraction: the material after the enzymatic conversion method adds above-mentioned solvent again, makes the garlic slurry be transferred to 1:9 with the weight of solvent ratio, input ultrasonic extraction unit, and ultrasonic frequency 25KHz handles 50min at normal temperature;
D. removal of impurities: centrifugal solid-liquid separates, after the secondary filter, carry out ultrafiltration, adopts ultra-filtration membrane to separate and removes macromolecular substance, and ultra-filtration membrane is a ceramic membrane, the ultra-filtration membrane molecular weight 30000Da that dams;
E. vacuum concentration: separate clear liquid and adopt the reverse osmosis concentration unit, membrane concentration makes solid content reach 30% at normal temperatures;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%.
Claims (1)
1. method for preparing garlicin from garlic is made of following steps:
A. after the garlic decortication, pulverize making beating;
B. enzymatic conversion method: alliin is transformed to garlicin;
C. ultrasonic extraction;
D. removal of impurities: after centrifugal solid-liquid separation, the secondary filter, carry out ultrafiltration, adopt ultra-filtration membrane to separate and removes macromolecular substance;
E. vacuum concentration: the clear liquid that obtains after the removal of impurities adopts the reverse osmosis concentration unit to carry out membrane concentration;
F. spray is done: concentrated extract places the lyophilize of lyophilize unit, and can obtain purity is the garlicin pulvis of 1-3%;
It is characterized in that:
Among the step b, as solvent, its concentration is 0-100% with the alcoholic acid aqueous solution, and garlic slurry and weight of solvent are than 1: 2-6 imports in the reactor, temperature of reaction 30-50 ℃, and reaction times 60-120min;
Among the step c, will add above-mentioned solvent in the material after the enzymatic conversion method again, make the garlic slurry be transferred to 1 with the weight of solvent ratio: 6-10, input ultrasonic extraction unit, ultrasonic frequency 25KHz handles 30-60min at normal temperature;
In the steps d, ultra-filtration membrane is mineral membrane or ceramic membrane, the ultra-filtration membrane molecular weight 8000-50000Da that dams;
Among the step e, concentrate at normal temperatures, be concentrated into solid content and reach 25-35%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101396000A CN101338329B (en) | 2008-08-28 | 2008-08-28 | Method for preparing garlicin from garlic |
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| CN2008101396000A CN101338329B (en) | 2008-08-28 | 2008-08-28 | Method for preparing garlicin from garlic |
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| CN101338329A CN101338329A (en) | 2009-01-07 |
| CN101338329B true CN101338329B (en) | 2011-02-09 |
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Families Citing this family (14)
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|---|---|---|---|---|
| GB0903869D0 (en) | 2009-03-05 | 2009-04-22 | Neem Biotech Ltd | Process for the preparation of ajoene |
| CN102499967B (en) * | 2011-11-18 | 2013-10-23 | 江苏大学 | Ultrasonic-assisted method for preparing garlic blood-pressure-lowering functional factors |
| CN102697048A (en) * | 2012-06-11 | 2012-10-03 | 邯郸市春风科技发展有限公司 | Method for extracting natural active substance in garlic by using ultrasonic wave |
| CN102850245B (en) * | 2012-09-04 | 2014-07-30 | 江苏大学 | Method for ultrasonic assisted extraction of alliin in garlic |
| CN103772771A (en) * | 2013-12-06 | 2014-05-07 | 苏州瑞邦塑胶有限公司 | Process for manufacturing bacteriostatic composite film from waste plastic and waste rubber |
| CN104151222A (en) * | 2014-07-18 | 2014-11-19 | 常州大学 | Method for extracting allicin |
| CN105475922B (en) * | 2015-09-23 | 2021-03-30 | 黑龙江省科学院 | Black potato and preparation method thereof |
| CN105146603B (en) * | 2015-09-23 | 2021-03-30 | 黑龙江省科学院 | Black chestnut and preparation method thereof |
| CN105166195A (en) * | 2015-09-23 | 2015-12-23 | 黑龙江省科学院 | Hemp herb tea |
| CN105231190A (en) * | 2015-09-23 | 2016-01-13 | 黑龙江省科学院 | Edible fructus cannabis raw materials, fructus cannabis fat and fructus cannabis protein powder as well as preparation methods thereof |
| CN105166928A (en) * | 2015-09-25 | 2015-12-23 | 黑龙江省科学院 | Anthocyanin and allicin integrated oral liquid and preparation method thereof |
| CN106957883A (en) * | 2017-04-06 | 2017-07-18 | 山东晨隆晟世生物科技有限公司 | A kind of allicin synthesizes the process of 4,5,9-trithiadodeca-1,6,11-triene 9-oxide |
| CN108147600A (en) * | 2017-10-18 | 2018-06-12 | 安徽国瑞食品有限公司 | A kind of method from dewatered garlic flake processing waste water effective component extracting |
| CN108703332A (en) * | 2018-06-05 | 2018-10-26 | 兰陵同源益民生物科技有限公司 | A kind of garlic cellulose product and preparation method thereof |
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Owner name: SHANDONG CHENNONG HEALTH INDUSTRY CO., LTD. Free format text: FORMER NAME: SHANDONG JUYE CHENENG NATURAL PRODUCT CO., LTD. |
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Address after: 274933 economic development zone, Dong Tun Town, Juye County, Heze, Shandong Patentee after: SHANDONG CHENNONG HEALTH INDUSTRY CO., LTD. Address before: 274933 economic development zone, Dong Tun Town, Juye County, Heze, Shandong Patentee before: Shandong Juye Cheneng Natural Product Co., Ltd. |
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Effective date of registration: 20180604 Address after: 274900 Yongfeng Road, Juye County, Heze, Shandong, north of Qilin Avenue (formerly Renmin Road) and Lin Tai Road. Patentee after: Shandong garlic Yuan Tang Bio Technology Co., Ltd. Address before: 274933 Economic Development Zone, Dong Guan Tun Town, Juye County, Heze, Shandong Patentee before: SHANDONG CHENNONG HEALTH INDUSTRY CO., LTD. |
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