CN106083681A - A kind of garlicin extraction process - Google Patents

A kind of garlicin extraction process Download PDF

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Publication number
CN106083681A
CN106083681A CN201610522014.9A CN201610522014A CN106083681A CN 106083681 A CN106083681 A CN 106083681A CN 201610522014 A CN201610522014 A CN 201610522014A CN 106083681 A CN106083681 A CN 106083681A
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China
Prior art keywords
garlicin
extraction process
mashed garlic
garlic
60min
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CN201610522014.9A
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Chinese (zh)
Inventor
谭秋苹
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CHENGDU SHENGHUI ELECTRONIC TECHNOLOGY Co Ltd
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CHENGDU SHENGHUI ELECTRONIC TECHNOLOGY Co Ltd
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Priority to CN201610522014.9A priority Critical patent/CN106083681A/en
Publication of CN106083681A publication Critical patent/CN106083681A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C381/00Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00

Abstract

The invention discloses a kind of garlicin extraction process.This technique comprises the following steps: (1) gets the raw materials ready: ripe, dry, the free from insect pests of hanking, without the Bulbus Allii gone rotten, stalk, point lobe, stripping underwear, rinses with clear water, removes impurity and undesirable set of garlic tablet;(2) pulverize: by the garlic tablet clean water selected by step (1), be subsequently processed into the particle diameter of the largest particles in mashed garlic, and mashed garlic and be less than 0.2mm;(3) extract: selecting mass fraction 95 98% ethanol is extractant, enzymolysis 20 60min placed at 20 40 DEG C by the mashed garlic of step (2), take 400 800ml extractants by 200g mashed garlic and extract 20 60min, obtain garlicin extracting solution, taking supernatant liquid filtering after garlicin extracting solution is centrifugal, filtrate is garlicin lixiviating solution;(4) purification: prepare pure garlicin by isolated and purified for garlicin lixiviating solution.Garlicin in Bulbus Allii can sufficiently be extracted by present invention process, improves the extraction ratio of garlicin.

Description

A kind of garlicin extraction process
Technical field
The present invention relates to a kind of garlicin extraction process.
Background technology
Bulbus Allii is the bulb of the raw Bulbus Allii of Liliaceae allium, originates in western part of Asia.China is the major country of production of Bulbus Allii, Annual production accounts for the 25% of Gross World Product, and the fresh Bulbus Allii of China and various fabricated product, in addition to supply domestic consumption, export day the most in a large number Basis and Southeast Asia.The Bulbus Allii of 80% in Japan and southeast asian market is China's export, but fresh Bulbus Allii rest period is short, Yi Fa Bud goes mouldy, not storage endurance, can cause huge waste;Bulbus Allii head product price is relatively low, if by Bulbus Allii deep processing, and particularly deodorize Bulbus Allii Element series of products are greatly improved its economic benefit.The finely processed product of Bulbus Allii has again storage endurance, facilitates the features such as transport, because of This, develop stink-free garlicin series of products wide market.Garlicin is main in perennial root draft liliaceous plant Bulbus Allii Wanting the general name of bioactive ingredients, being used as medicine in China has long history, is a kind of broad spectrum antibiotic, has antiinflammatory, blood pressure lowering, fall Blood fat, suppress Platelet congregation, reduce coronary atherosclerosis, suppress the synthesis of internal N nitrosamine, anti-cancer, for cancer, antiviral etc. Multiple efficacies.Garlicin reaches 80%--95% as people's medicine to respiratory tract, digestive tract, meningitis, intestinal tract disease effective percentage, also may be used As veterinary drug, pesticide and food additive etc..Garlicin, can be as antibacterial, insecticide, antidote, seasoning in feedstuff Agent, animal health increasing agent and quality improving agent.Therefore, the research tool of garlicin is of great significance.
The content of garlicin is main and kind, growth and development stage, organ, position, condition of storage, storage time, process The factors such as method, pH value, temperature, cultivation condition are relevant.The difference of its Allicin Content of Bulbus Allii of different cultivars be by heredity The difference of characteristic determines;And the Bulbus Allii of same kind is at different growth and development stages and same growth and development stage not With organ and different parts, and, Bulbus Allii is under the different storage time, and its alliin is different with allinase activity, Bulbus Allii Cellulose content also differs;It addition, use different processing extracting method, sulfur-containing compound in Bulbus Allii can be caused different breaking Bad, and due to the difference of extraction degree, will also result in the difference of Allicin Content.
Summary of the invention
The technical problem to be solved is to provide a kind of garlicin extraction process, and this preparation technology can be sufficient Garlicin in Bulbus Allii is extracted, improves the extraction ratio of garlicin, in order to improve commercial Application and industrialization produces The economic benefit brought.
The present invention solves above-mentioned technical problem and be the technical scheme is that a kind of garlicin extraction process, including following Step:
(1) get the raw materials ready: ripe, dry, the free from insect pests of hanking, without the Bulbus Allii gone rotten, stalk, point lobe, stripping underwear, rinse with clear water, Remove impurity and undesirable set of garlic tablet;
(2) pulverize: by the garlic tablet clean water selected by step (1), be subsequently processed in mashed garlic, and mashed garlic maximum The particle diameter of grain is less than 0.2mm;
(3) extract: selecting mass fraction 95-98% ethanol is extractant, and the mashed garlic of step (2) is placed at 20-40 DEG C Enzymolysis 20-60min, takes 400-800ml extractant by 200g mashed garlic and extracts 20-60min, obtain garlicin extracting solution, and garlicin carries Taking after liquid is centrifuged and take supernatant liquid filtering, filtrate is garlicin lixiviating solution;
(4) purification: prepare pure garlicin by isolated and purified for garlicin lixiviating solution.
Present invention generally provides a kind of preparation technology fully extracted from Bulbus Allii by garlicin, extract acquisition Garlicin lixiviating solution the most isolated and purified, the technical scheme preparing pure garlicin is existing, uses existing purification side Method can obtain pure garlicin.
Specifically, also include soaking deodorization step before described pulverising step: the garlic tablet of step (1) gained is immersed deodorant liquid Middle immersion 20-30h, deodorant liquid be mass percent be the fumaric acid solution of 2.5-3.5%, or deodorant liquid is anti-butylene Diacid, acetic acid mixed solution, in mixed solution, the mass percent of fumaric acid solution is 2.5-3.5%, the quality of acetic acid Percentage ratio is 1.5-3.0%.
In described step (2), the particle diameter of mashed garlic the largest particles is less than 0.1mm.
The mass fraction 96-98% of ethanol in the extraction process of described step (3).
Further, the mass fraction 98% of ethanol in the extraction process of described step (3).
In the extraction process of described step (3), enzymolysis 40-60min placed at 20-30 DEG C by the mashed garlic of step (2).
Further, in the extraction process of described step (3), enzymolysis 60min placed at 30 DEG C by the mashed garlic of step (2).
In the extraction process of described step (3), take 600-800ml extractant by 200g mashed garlic and extract 40-60min.
Further, in the extraction process of described step (3), take 600ml extractant by 200g mashed garlic and extract 60min.
The invention has the beneficial effects as follows: this optimum preparation condition extracting method, can sufficiently by the Bulbus Allii in Bulbus Allii Element extracts, and improves the extraction ratio of garlicin, in order to improve commercial Application and industrialization produces the economic benefit brought.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited only to This.
Embodiment:
1, experiment material
The 1.1 common commercially available Bulbus Alliis of vegetable material
1.2 key instrument equipment
Desk centrifuge thermostat water bath baking oven pulverizer electronics Libra electric furnace
1.3 main agents
98% ethanol concentrated hydrochloric acid sodium hydroxide barium chloride methyl orange
2, experimental technique
2.1 technological process
Garlic raw material → broken → extraction → separation → garlicin lixiviating solution → purification.
2.2 detailed steps:
2.2.1 get the raw materials ready.Hank ripe, dry, free from insect pests, without the Bulbus Allii gone rotten, stalk, point lobe, stripping underwear, float with clear water Wash, remove impurity and undesirable set of garlic tablet.
2.2.2, deodorization is soaked: the garlic tablet of 2.2.1 gained immersed in deodorant liquid and soak 20-30h.Deodorant liquid is quality hundred Proportion by subtraction is the fumaric acid solution of 2.5-3.5%;Or, deodorant liquid is fumaric acid, acetic acid mixed solution, mixed solution The mass percent of middle fumaric acid solution is 2.5-3.5%, and the mass percent of acetic acid is 1.5-3.0%.
2.2.3, broken.It is processed into mashed garlic with pulverizer after the garlic tablet clean water that will obtain in 2.2.2.(due to not Pulverize completely, grind again once with mortar, make as far as possible mashed garlic exists without bigger granule, the particle diameter of the largest particles in mashed garlic Less than 0.2mm, it is desirable to little Yu 0.1mm)
Measure variable concentrations the most respectively, the mashed garlic weighed is extracted by the ethanol of different volumes, extraction one timing After between, pouring 100ml centrifuge tube centrifugal 5min under 1400rpm into, then take supernatant, filter, filtrate is the garlicin at initial stage Lixiviating solution.By measuring the content of contained garlicin in garlicin lixiviating solution, the most different extraction processes is for garlicin Extraction degree, compares the garlicin extraction process drawing optimization.
Under different condition, Bulbus Allii is carried out the impact of deodorization
Process combination number Fumaric acid (%) Acetic acid (%)
1 2.5 0
2 2.8 0
3 0 1.5
4 0 2.3
5 2.5 1.5
6 2.8 2.3
7 3.0 2.6
8 3.2 2.8
9 3.5 3.0
According to the measurement result of upper table, in each deodorize processing scheme, deodorising effect is followed successively by from excellent to bad: 6 > 7 > 8 > 5 > 9 > 2 > 1 > 4 > 3, experiment shows, when deodorant liquid is fumaric acid, acetic acid mixed solution, deodorizing effect is best, is significantly higher than and only makes With fumaric acid or simply use the acetic acid effect as deodorant liquid, use the mixing of fumaric acid, acetic acid at deodorant liquid During solution, when in mixed solution, the mass percent of fumaric acid solution is 2.8%, and the mass percent of acetic acid is 2.3% Time deodorizing effect optimal.
Using the mass percent of fumaric acid solution in mixed solution is 2.8%, and the mass percent of acetic acid is After the scheme deodorization that when 2.3%, deodorizing effect is optimal, the extraction of garlicin is made further research by various extracting conditions.
Orthogonal table selected by this experiment and subordinate list L9 (3 thereof4):
Indicate that 9 groups of experiments, 9 groups of experiments are to carry out under the combination of 3 level 4 factors.
For examination factor and level
According to orthogonal experiment decomposition method, measuring can be carried out by following combination when 4 factor 3 level:
Owing to experimentation easily causing error, therefore measure two groups and average as measurement result.And, laboratory Volumetric flask minimum volume used is 50ml, and therefore, after filtering, garlicin lixiviating solution is less than instilling 98% second in the sample of 50ml Alcohol is dissolved to 50ml, is easy to next step calculating when measuring Allicin Content in garlicin lixiviating solution.
The mensuration of 2.3 Allicin Contents
Extract (or sample) 5m1 that Fix sulfur method mensuration Allicin Content takes containing garlicin is placed in small beaker, adds dense Nitric acid 2m1, stirring and evenly mixing, 20min is at room temperature placed to yellow, in the volumetric flask with distillation washing people 100m1, it is fixed to shake up Holding, accurately measure 80m1, add 0.1% methyl orange solution 5, being adjusted to solution with 10% sodium hydroxide is yellow, then with 18% Hydrochloric acid be adjusted to redness, and add 1m1, making solution is acidity, is put heating in sand bath and is concentrated into 50m1, and in 500W electric furnace After upper micro-boiling, adding 5% barium chloride solution lo ml. and shake up, 90 DEG C of water bath heat preservation 2h, quantitative filter paper filters, rushes with hot distilled water To without chloride ion (washing lower liquid can not make silver nitrate solution generate precipitation). it is known that the barium sulfate precipitate leached by filter paper merges old friend In the Citrus chachiensis Hort. snail of weight, after drying and make filter paper carbonization on 500W electric furnace.Move to calcination on 2000W electric furnace bleach (about to ash 30min), cooling, weigh, be calculated as follows the content of garlicin according to the weight of barium sulfate.
In formula: the molecular weight of 32.06 sulfur;233.39 barium sulfate molecular weight;A barium sulfate quality (g); 162.26 the molecular weight of garlicin;The grams (or milliliter number) of W sample (or extract);V measures extracting solution Milliliter number;V0Extracting solution cumulative volume milliliter number.
1. measure with Fix sulfur method according to formula.According to practical situation, by formula 1. based in the case of, according to formula 1. principle has done trickle adjustment.Concrete determination step is as follows:
2.3.1 measure garlicin lixiviating solution 5ml, add concentrated nitric acid 2ml, stir, fully react 30min, with distillation Wash in 50ml volumetric flask, be dissolved to 50ml stand-by.
The most upwards dripping 0.1% methyl orange 4 in step gained solution, it is yellow that 10% sodium hydroxide is adjusted to solution, then Being adjusted to redness with the hydrochloric acid of 18%, add 1m1, making solution is acidity.
2.3.3 add 10% barium chloride solution 5ml, put in 90 DEG C of water-baths and fully react 2h.
2.3.4 the upper reacted solution of step gained is filtered, with hot distilled water punching to (washing lower liquid without chloride ion and can not make nitre Acid silver solution generates precipitation).The barium sulfate precipitate leached by filter paper closes in the crucible putting into known weight together with filter paper, in Dry on 500W electric furnace, and after making filter paper carbonization. move to calcination on 2000W electric furnace and bleach to ash, cooling, weigh, according to sulfur The weight of acid barium is calculated as follows the content of garlicin.For reducing experimental error, measure an air filter paper calcination to after ash Quality makees reference.
It is after simplification:
In formula: the molecular weight of 32.06 sulfur;233.39 barium sulfate molecular weight;A barium sulfate quality (g);162.26— The molecular weight of garlicin;W garlicin sample quality (g);V measures extracting solution milliliter number;V0 extracting solution cumulative volume Milliliter number.
2.4 experimental result
Being computed, in the garlicin extracting solution of two groups of process specimen in use mashed garlic, Allicin Content is as shown in the table (following Data are two groups of averages processing data):
Combination number Example garlic shale amount (g) Allicin Content (‰)
1 19.942 3.82
2 20.406 3.58
3 19.855 3.20
4 20.655 3.50
5 20.089 3.11
6 19.870 2.74
7 20.299 2.80
8 18.625 2.43
9 19.944 2.30
According to the measurement result of upper table, each garlicin processed extracts Allicin Content in night and is followed successively by from big to small: 1 > 2 > 4 > 3 > 5 > 7 > 6 > 8 > 9, experiment shows, the concentration of alcohol of extraction used is the highest, measures gained Allicin Content higher, and it is right to illustrate Garlicin extracts the most abundant;It is the longest that enzymolysis time placed by mashed garlic, and garlicin extraction ratio is the highest;Add the volume of ethanol extract The most, the highest to garlicin extraction ratio;Addition ethanol extract extraction time is the longest, and garlicin extraction ratio is the highest.
Therefore, selecting 98% ethanol is extractant, places enzymolysis 60min, take 60ml98% second by 20g mashed garlic at 30 DEG C Alcohol is the technique that extractant extracts 60min, and the extraction to garlicin is the most abundant.
The above, be only presently preferred embodiments of the present invention, and the present invention not does any pro forma restriction, every depends on According to the technical spirit of the present invention, any simple modification that above example is made, equivalent variations, each fall within the protection of the present invention Within the scope of.

Claims (9)

1. a garlicin extraction process, it is characterised in that comprise the following steps:
(1) get the raw materials ready: ripe, dry, the free from insect pests of hanking, without the Bulbus Allii gone rotten, stalk, point lobe, stripping underwear, rinse with clear water, remove Impurity and undesirable set of garlic tablet;
(2) pulverize: by the garlic tablet clean water selected by step (1), be subsequently processed into the largest particles in mashed garlic, and mashed garlic Particle diameter is less than 0.2mm;
(3) extract: selecting mass fraction 95-98% ethanol is extractant, and enzymolysis placed at 20-40 DEG C by the mashed garlic of step (2) 20-60min, takes 400-800ml extractant by 200g mashed garlic and extracts 20-60min, obtain garlicin extracting solution, garlicin extracting solution Taking supernatant liquid filtering after Li Xin, filtrate is garlicin lixiviating solution;
(4) purification: prepare pure garlicin by isolated and purified for garlicin lixiviating solution.
A kind of garlicin extraction process the most according to claim 1, it is characterised in that in described step (2), mashed garlic is maximum The particle diameter of granule is less than 0.1mm.
A kind of garlicin extraction process the most according to claim 1, it is characterised in that the extraction process of described step (3) The mass fraction 96-98% of middle ethanol.
A kind of garlicin extraction process the most according to claim 3, it is characterised in that the extraction process of described step (3) The mass fraction 98% of middle ethanol.
A kind of garlicin extraction process the most according to claim 1, it is characterised in that the extraction process of described step (3) In, enzymolysis 40-60min placed at 20-30 DEG C by the mashed garlic of step (2).
A kind of garlicin extraction process the most according to claim 5, it is characterised in that the extraction process of described step (3) In, enzymolysis 60min placed at 30 DEG C by the mashed garlic of step (2).
A kind of garlicin extraction process the most according to claim 1, it is characterised in that the extraction process of described step (3) In, take 600-800ml extractant by 200g mashed garlic and extract 40-60min.
A kind of garlicin extraction process the most according to claim 7, it is characterised in that the extraction process of described step (3) In, take 600ml extractant by 200g mashed garlic and extract 60min.
A kind of garlicin extraction process the most according to claim 1, it is characterised in that also include leaching before described pulverising step Bubble deodorization step: the garlic tablet of step (1) gained is immersed and soaks 20-30h in deodorant liquid, deodorant liquid be mass percent be 2.5- The fumaric acid solution of 3.5%, or deodorant liquid is fumaric acid, acetic acid mixed solution, anti-butylene two in mixed solution The mass percent of acid solution is 2.5-3.5%, and the mass percent of acetic acid is 1.5-3.0%.
CN201610522014.9A 2016-06-30 2016-06-30 A kind of garlicin extraction process Pending CN106083681A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106613266A (en) * 2016-12-30 2017-05-10 山东农业大学 Method for relieving apple continuous cropping obstacles by means of allicin
CN107616504A (en) * 2017-10-23 2018-01-23 何正国 A kind of beneficial allicin biological synthesis method
CN108013258A (en) * 2017-11-20 2018-05-11 锦州景良动物药业有限公司 A kind of preparation method of the livestock fodder additives containing allicin
CN111938025A (en) * 2020-08-12 2020-11-17 广州快大饲料有限公司 Plant extract additive for livestock and poultry breeding
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
CN113924287A (en) * 2019-05-29 2022-01-11 澳大利亚大蒜生产商私人有限公司 Health product from garlic green top

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106613266A (en) * 2016-12-30 2017-05-10 山东农业大学 Method for relieving apple continuous cropping obstacles by means of allicin
CN107616504A (en) * 2017-10-23 2018-01-23 何正国 A kind of beneficial allicin biological synthesis method
CN108013258A (en) * 2017-11-20 2018-05-11 锦州景良动物药业有限公司 A kind of preparation method of the livestock fodder additives containing allicin
CN113924287A (en) * 2019-05-29 2022-01-11 澳大利亚大蒜生产商私人有限公司 Health product from garlic green top
CN111938025A (en) * 2020-08-12 2020-11-17 广州快大饲料有限公司 Plant extract additive for livestock and poultry breeding
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

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