CN106337070A - Garlicin extraction method - Google Patents
Garlicin extraction method Download PDFInfo
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- CN106337070A CN106337070A CN201610717030.3A CN201610717030A CN106337070A CN 106337070 A CN106337070 A CN 106337070A CN 201610717030 A CN201610717030 A CN 201610717030A CN 106337070 A CN106337070 A CN 106337070A
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- garlicin
- bulbus allii
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- enzymolysis
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P11/00—Preparation of sulfur-containing organic compounds
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Abstract
The invention provides a garlicin extraction method, which comprises the steps of pretreatment, enzymatic hydrolysis, extraction and vacuum concentration. According to the invention, heat generated by microwave radiation is used for effecting in garlic tissue, alliin in the cells flows out from the cell wall, then enzymatic hydrolysis and catalysis are carried out for conversing alliin to garlicin, moisture content of a garlic sample is greatly reduced through freeze drying, subsequent ethanol extraction is convenient, a whole process is carried out orderly, the recovery rate is high, stability is good; finally through vacuum concentration, a leaching liquor ethanol is removed, cost is low, no harmful solvent residues is generated, and the method is suitable for industrial production.
Description
Technical field
The present invention relates to effective ingredients in plant extracts field, particularly to a kind of extracting method of garlicin.
Background technology
Bulbus Allii is a kind of plant of dietotherapeutic, belongs to for Liliaceae Allium, and its bulb is not only rich in calcium, phosphorus, ferrum, zinc and germanium
With the inorganic elementss such as selenium, and be rich in multiple essential amino acids；Additionally, being also rich in organic sulfur compound, flavonoid class compound, many
Sugar and saponins compound isoreactivity composition.It is in the aspects such as anti-inflammation, antiviral, blood pressure lowering, antioxidation, blood fat reducing all tables
Reveal good result.In the numerous active component of Bulbus Allii, the most notable with effect of garlicin.Garlicin is allicin, big
Bulbus Allii is newly plain and the general name of multiple allylic thioether compound, and chemical name is diallyl trisulfide (dats), and molecular formula is
c6h10s3.It is a kind of colorless oil with off-odor and highly volatile, chemical composition be mainly allyl sulphide and
Thioester compound, such as Diallytrisin, diallyl disulphide and GIUCOSinoate.Fresh big
There is no free garlicin, only its precursor substance alliin, alliin is presented in stable in Bulbus Allii in Bulbus Allii
In, after Bulbus Allii is subject to physics or Mechanical Crushing, the oxygen molecule of in the air has caused the alliin together with associating with Bulbus Allii former times enzyme
Resolve into garlicin.
Garlicin has antimicrobial, parasiticide, antitumor, defying age, antiulcer, improves immunity of organisms etc. in many ways
Face pharmacological action, additionally can remove the fat accumulating in the blood vessel, have obvious reduction Triglycerides in Serum and total gallbladder
The effect of sterin content, the content that HDL-C can be improved simultaneously and reduce low-density lipoprotein cholesterol,
And by reducing blood viscosity, the occurrence and development of suppression atherosclerotic lesion.Therefore, the research of garlicin and opening
Send out and also more and more paid attention to by people.
Extracting method with regard to garlicin mainly has steam distillation, supercritical fluid extraction and has both at home and abroad at present
Machine solvent extraction method.Steam distillation is one of most common method, and it has, and equipment is simple, low cost, good stability etc.
Feature, but because fermentation and vapo(u)rizing temperature are of a relatively high, the activity decrease of allinase, garlicin extraction ratio is relatively low, main
To be the diallyl sulfide that garlicin is degraded further；Supercritical fluid extraction operation temperature is low, although products therefrom
Based on garlicin, but equipment one-time investment is larger, and loading and unloading all adopts batch (-type), and experimental facilitiess have high demands；Solvent extraction
The solvent that method uses mostly is ether, but its volatility is larger, and has certain toxicity.Ethanol is with its safe and nontoxic and one-tenth
This cheap advantage becomes the best substitute of ether, but prior art often extraction ratio less than 0.2%.
How to develop a kind of new technology, on the basis of not increasing cost, improving garlicin extraction ratio is that we currently need
Problem to be considered.
Content of the invention
The main object of the present invention is that and overcomes weak point of the prior art, provides that a kind of equipment is simple, extracts
The high garlicin extracting method of rate.
The present invention proposes a kind of extracting method of garlicin, comprises the steps:
S10, pretreatment: take fresh garlic, be pounded mashed garlic with tissue mashing machine after peeled wash, plus deionized water stirring is all
Use 200w microwave radiation 2 5min after even, obtain Bulbus Allii serosity；
S20, enzymolysis: adjust Bulbus Allii serosity ph value for being placed in 30 45 DEG C of water-baths after 45 with the hydrochloric acid that concentration is 15%
Lyophilization 6h after middle enzymolysis 0.5 2h, obtains treatment fluid；
S30, extraction: add the ethanol that volume fraction is 90% to extract 0.8 1.2h at 30 50 DEG C toward in treatment fluid,
After 3500r/min is centrifuged 10 15min, take supernatant liquid filtering；Wherein the quality for the treatment of fluid and the ratio of ethanol volume are 1g:5ml；
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, the condition of rotating speed 75r/min
Under, carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin concentrating.
Preferably, in step s20, Bulbus Allii serosity adjusts through hydrochloric acid and is placed in enzymolysis 0.5h in 40 DEG C of water-baths after ph value.
The heat effect that technical solution of the present invention produces first with microwave radiation, in the organization internal of Bulbus Allii, makes positioned at intracellular
Alliin flow out from cell wall, then enzymolysis catalysis alliin is converted into garlicin, and is greatly reduced by lyophilization
The moisture of garlic samples, facilitates subsequent ethanol to extract, whole process is carried out in order, extraction ratio is high, good stability；Finally lead to
Cross concentrating under reduced pressure, remove lixiviating solution ethanol, low cost, no hazardous solvent remain, suitable industrialized production.
Specific embodiment
It should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention
Scope.
The present invention proposes a kind of extracting method of garlicin, comprises the steps:
S10, pretreatment: take fresh garlic, be pounded mashed garlic with tissue mashing machine after peeled wash, plus deionized water stirring is all
Use 200w microwave radiation 2 5min after even, obtain Bulbus Allii serosity；
The heat effect being produced using microwave radiation in Bulbus Allii vascular tissue internal so as in vascular bundle and glandular cell's system
Very fast intensification, and this temperature can be kept until its internal pressure exceedes the ability of cell wall expansion, cause cell rupture, thus
Make to flow out from cell wall positioned at intracellular alliin, the serosity that transmits and transfer to surrounding, facilitate follow-up enzymolysis step.
S20, enzymolysis: adjust Bulbus Allii serosity ph value for being placed in 30 45 DEG C of water-baths after 45 with the hydrochloric acid that concentration is 15%
Lyophilization 6h after middle enzymolysis 0.5 2h, obtains treatment fluid；
The step of enzymolysis is to promote alliin to convert to garlicin.After Garlic cell crushes, produce allinase, promote Bulbus Allii
Propylhomoserin converts to garlicin.Preferably, 40 DEG C of water-baths are placed 0.5h.Hydrolysis temperature is too low, and the activity of allinase is little,
The time that catalysis alliin is converted into garlicin is oversize；And temperature is too high, the garlicin of generation is easy to decompose again.Enzymolysis time
Too short, alliin can not be sufficiently converted into garlicin；And enzymolysis time is long, garlicin is readily volatilized or is converted into by-product,
Impact yield and quality.Thus when temperature is 40 DEG C, when enzymolysis time is 0.5h, the yield highest of garlicin.
The yield of the garlicin of freeze-dried process greatly improves, and main cause is that lyophilization can greatly reduce greatly
The moisture of Bulbus Allii sample, is conducive to subsequently extracting.
S30, extraction: add the ethanol that volume fraction is 90% to extract 0.8 1.2h at 30 50 DEG C toward in treatment fluid,
After 3500r/min is centrifuged 10 15min, take supernatant liquid filtering；Wherein the quality for the treatment of fluid and the ratio of ethanol volume are 1g:5ml；
During centrifugation, rotating speed was advisable with 10 15min with 3500r/min, time.If speed is excessively slow, centrifugation can be made not thorough；
Too fast, garlicin dissolving can be caused insufficient.
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, the condition of rotating speed 75r/min
Under, carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin concentrating.
This step is used for removing lixiviating solution ethanol.
The garlicin extracting can measure content using Fix sulfur method, and method is as follows:
Take the 5ml of sample containing garlicin to be placed in small beaker, add concentrated nitric acid 2ml, stirring and evenly mixing is to yellow.Put at room temperature
Put 20min, washed with distilled water in the volumetric flask of 100ml, shake up constant volume, accurately measure 80ml, add 0.1% methyl orange solution
5, being adjusted to solution with 10% sodium hydroxide solution is in yellow, then is adjusted to redness with 18% hydrochloric acid, and adds 1ml, makes solution
In acidity, put in sand bath heating and be concentrated into 50ml, and after micro-boiling on the 500w electric furnace, added 5% barium chloride solution 10ml,
Shake up, 90 DEG C of water bath heat preservation 2h, quantitative filter paper filters, and rushes to no chloride ion with hot distilled water that (washing lower liquid can not make silver nitrate molten
Liquid generates precipitation).The barium sulfate precipitate merging that filter paper is leached is put into oneself and is known in the crucible of weight, dries on 500w electric furnace,
And after making filter paper carbonization, move to calcination to ash on 2000w electric furnace and bleach (about 30min), cooling is weighed, according to the weight of barium sulfate
Amount is calculated as follows the content of garlicin.
In formula: 32.06 is the molecular weight of sulfur；233.39 being barium sulfate molecular weight；162.26 the molecular weight for garlicin；a
For barium sulfate quality (g)；W is the volume (ml) of sample；V is to measure extracting liquid volume (ml)；v1For extracting solution cumulative volume (ml).
Embodiment 1:
S10, pretreatment: take fresh garlic 200g, after peeled wash, be pounded mashed garlic with tissue mashing machine, plus deionized water
500g uses 200w microwave radiation 4min after stirring, and obtains Bulbus Allii serosity 640g；
S20, enzymolysis: the hydrochloric acid 400ml being 15% with concentration adjusts Bulbus Allii serosity ph value for being placed in 30 DEG C of water-baths after 4
Lyophilization 6h after enzymolysis 1.8h；
S30, extraction: add the ethanol 5l that volume fraction is 90% to extract 1h at 35 DEG C, 3500r/min is centrifuged 15min
Afterwards, take supernatant liquid filtering；
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, the condition of rotating speed 75r/min
Under, carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin concentrating.
It is 0.315% that the garlicin obtaining adopts Fix sulfur method to measure content.
Embodiment 2:
S10, pretreatment: take fresh garlic 300g, after peeled wash, be pounded mashed garlic with tissue mashing machine, plus deionized water
600g uses 200w microwave radiation 2min after stirring, and obtains Bulbus Allii serosity 860g；
S20, enzymolysis: the hydrochloric acid 520ml being 15% with concentration adjusts Bulbus Allii serosity ph value for being placed in 40 DEG C of water-baths after 5
Lyophilization 6h after enzymolysis 0.5h；
S30, extraction: add the ethanol 6.8l that volume fraction is 90% to extract 0.8h at 30 DEG C, 3500r/min is centrifuged
After 10min, take supernatant liquid filtering；
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, the condition of rotating speed 75r/min
Under, carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin concentrating.
It is 0.396% that the garlicin obtaining adopts Fix sulfur method to measure content.
Embodiment 3:
S10, pretreatment: take fresh garlic 100g, after peeled wash, be pounded mashed garlic with tissue mashing machine, plus deionized water
200g uses 200w microwave radiation 5min after stirring, and obtains Bulbus Allii serosity 280g；
S20, enzymolysis: the hydrochloric acid 120ml being 15% with concentration adjusts Bulbus Allii serosity ph value for being placed in 38 DEG C of water-baths after 4.5
Lyophilization 6h after middle enzymolysis 2h；
S30, extraction: add the ethanol 2l that volume fraction is 90% to extract 1.2h at 50 DEG C, 3500r/min is centrifuged
After 12min, take supernatant liquid filtering；
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, the condition of rotating speed 75r/min
Under, carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin concentrating.
It is 0.342% that the garlicin obtaining adopts Fix sulfur method to measure content.
The extraction process of the present invention can more effectively extract the garlicin in Bulbus Allii, and content can reach 0.396%.
And technological operation is simple, reasonable, provide foundation for further large-scale production.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (2)
1. a kind of extracting method of garlicin is it is characterised in that comprise the steps:
S10, pretreatment: take fresh garlic, after peeled wash, be pounded mashed garlic with tissue mashing machine, plus after deionized water stirs
With 200w microwave radiation 2 5min, obtain Bulbus Allii serosity；
S20, enzymolysis: adjust Bulbus Allii serosity ph value for being placed in enzyme in 30 45 DEG C of water-baths after 45 with the hydrochloric acid that concentration is 15%
Solve lyophilization 6h after 0.5 2h, obtain treatment fluid；
S30, extraction: add the ethanol that volume fraction is 90% to extract 0.8 1.2h at 30 50 DEG C toward in treatment fluid,
After 3500r/min is centrifuged 10 15min, take supernatant liquid filtering；Wherein the quality for the treatment of fluid and the ratio of ethanol volume are 1g:5ml；
S40, concentrating under reduced pressure: the supernatant after filtration is 50 DEG C in temperature, pressure 0.01mpa, under conditions of rotating speed 75r/min,
Carry out concentrating under reduced pressure with Rotary Evaporators, obtain the garlicin extracting.
2. the extracting method of garlicin as claimed in claim 1 is it is characterised in that in step s20, Bulbus Allii serosity is adjusted through hydrochloric acid
It is placed in enzymolysis 0.5h in 40 DEG C of water-baths after section ph value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610717030.3A CN106337070A (en) | 2016-08-24 | 2016-08-24 | Garlicin extraction method |
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| CN201610717030.3A CN106337070A (en) | 2016-08-24 | 2016-08-24 | Garlicin extraction method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342421A (en) * | 2018-02-11 | 2018-07-31 | 常德金德新材料科技股份有限公司 | A kind of allicin extracting method |
| CN109198043A (en) * | 2018-09-10 | 2019-01-15 | 湖南常德九品福绿色食品有限公司 | The novel preparation method of garlic multipurpose oil |
| CN110305053A (en) * | 2019-05-20 | 2019-10-08 | 长沙学院 | A kind of hydrochloric ultrasonic wave wave extracts the method and garlic powder of allicin |
| CN110643433A (en) * | 2019-09-17 | 2020-01-03 | 武汉市赟巨科技有限公司 | Extraction method of dendrobium flower essential oil |
| CN112322671A (en) * | 2020-11-02 | 2021-02-05 | 江苏黎明食品集团有限公司 | Garlic water extract for promoting intestinal evacuation |
| CN114703239A (en) * | 2022-03-22 | 2022-07-05 | 辰欣药业股份有限公司 | Production method of allicin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683332A (en) * | 2005-03-15 | 2005-10-19 | 中国农业大学 | Method for extracting garlicin |
| CN103229881A (en) * | 2013-05-10 | 2013-08-07 | 北京绿源求证科技发展有限责任公司 | Heart nourishing food health-care tea electuary |
| CN103436564A (en) * | 2013-09-12 | 2013-12-11 | 南京泽朗农业发展有限公司 | Method for extracting allicin by using microwave-ultrasonic wave |
| CN103564197A (en) * | 2013-11-13 | 2014-02-12 | 福建正源饲料有限公司 | Compound plant extract feed additive and preparation method thereof |
-
2016
- 2016-08-24 CN CN201610717030.3A patent/CN106337070A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683332A (en) * | 2005-03-15 | 2005-10-19 | 中国农业大学 | Method for extracting garlicin |
| CN103229881A (en) * | 2013-05-10 | 2013-08-07 | 北京绿源求证科技发展有限责任公司 | Heart nourishing food health-care tea electuary |
| CN103436564A (en) * | 2013-09-12 | 2013-12-11 | 南京泽朗农业发展有限公司 | Method for extracting allicin by using microwave-ultrasonic wave |
| CN103564197A (en) * | 2013-11-13 | 2014-02-12 | 福建正源饲料有限公司 | Compound plant extract feed additive and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342421A (en) * | 2018-02-11 | 2018-07-31 | 常德金德新材料科技股份有限公司 | A kind of allicin extracting method |
| CN109198043A (en) * | 2018-09-10 | 2019-01-15 | 湖南常德九品福绿色食品有限公司 | The novel preparation method of garlic multipurpose oil |
| CN109198043B (en) * | 2018-09-10 | 2022-03-08 | 湖南常德九品福绿色食品有限公司 | Novel preparation method of garlic multipurpose oil |
| CN110305053A (en) * | 2019-05-20 | 2019-10-08 | 长沙学院 | A kind of hydrochloric ultrasonic wave wave extracts the method and garlic powder of allicin |
| CN110643433A (en) * | 2019-09-17 | 2020-01-03 | 武汉市赟巨科技有限公司 | Extraction method of dendrobium flower essential oil |
| CN112322671A (en) * | 2020-11-02 | 2021-02-05 | 江苏黎明食品集团有限公司 | Garlic water extract for promoting intestinal evacuation |
| CN114703239A (en) * | 2022-03-22 | 2022-07-05 | 辰欣药业股份有限公司 | Production method of allicin |
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Application publication date: 20170118 |