CN106187845A - The pre-treatment deodorizing method of garlicin extraction process - Google Patents
The pre-treatment deodorizing method of garlicin extraction process Download PDFInfo
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- CN106187845A CN106187845A CN201610519258.1A CN201610519258A CN106187845A CN 106187845 A CN106187845 A CN 106187845A CN 201610519258 A CN201610519258 A CN 201610519258A CN 106187845 A CN106187845 A CN 106187845A
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- garlicin
- extraction process
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C381/00—Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00
Abstract
The invention discloses the pre-treatment deodorizing method of a kind of garlicin extraction process.The method 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) soak deodorization: the garlic tablet of step (1) gained immersed in deodorant liquid and soak 20 30h, deodorant liquid be mass percent be the fumaric acid solution of 2.5 3.5%；(3) extraction purification: garlic tablet clean water step (2) soaked, is subsequently processed into mashed garlic, and the garlicin extracted in mashed garlic obtains garlicin extracting solution, is then peeled off purification, prepares pure garlicin.The deodorizing method of the present invention has preferable deodorising effect, and can be effectively retained garlicin while deodorize.
Description
Technical field
The present invention relates to the pre-treatment deodorizing method of 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 deodorize of garlicin is one of important step of garlicin application, only after deodorize processes garlicin system
Product just have practical value.Due to garlicin character extremely unstable, and the deodorize of untreated Bulbus Allii is easier, but should take off
The bioactive substances such as smelly reservation superoxide dismutase (SOD) the most as much as possible, garlicin are the most extremely difficult.
Summary of the invention
The technical problem to be solved is to provide the pre-treatment deodorizing method of a kind of garlicin extraction process, should
Method has preferable deodorising effect, and can be effectively retained garlicin while deodorize.
The present invention solves the pre-treatment deodorization side of above-mentioned technical problem the technical scheme is that garlicin extraction process
Method, 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, and stalk, point lobe, stripping underwear, with clear
Water rinses, and removes impurity and undesirable set of garlic tablet；(2) deodorization is soaked: the garlic tablet of step (1) gained immersed in deodorant liquid and soak
Bubble 20-30h, deodorant liquid be mass percent be the fumaric acid solution of 2.5-3.5%；(3) extraction purification: by step (2)
The garlic tablet clean water soaked, is subsequently processed into mashed garlic, and the garlicin extracted in mashed garlic obtains garlicin extracting solution, then divides
From purification, prepare pure garlicin.In this programme, the extraction purification of step (3) can use existing extraction and purification
Method realizes, and this programme is provided solely for the processing method of a kind of preferable deodorization.
Further, the deodorant liquid in described step (2) is fumaric acid, acetic acid mixed solution, anti-in mixed solution
The mass percent of butene dioic acid solution is 2.5-3.5%, and the mass percent of acetic acid is 1.5-3.0%.
In described step (2), the mass percent of fumaric acid solution is 2.5-3.0%.
The mass percent of described fumaric acid solution is 2.8%.
In described step (2), soak time is 22-25h.
In described step (2), soak time is 24h.
In described step (2), the mass percent of acetic acid is 2.0-2.5%.
In described step (2), the mass percent of acetic acid is 2.3%.
As the method for optimizing of extraction purification, concretely comprising the following steps of described step (3) extraction purification: select mass fraction
98% ethanol is extractant, and enzymolysis 60min placed at 30 DEG C by mashed garlic, takes 600ml extractant by 200g mashed garlic and extracts 60min,
Obtaining garlicin extracting solution, take supernatant liquid filtering after garlicin extracting solution is centrifugal, filtrate is garlicin lixiviating solution, is soaked by garlicin
Extract is isolated and purified prepares pure garlicin.
The invention has the beneficial effects as follows: the deodorizing method of the present invention has a preferable deodorising effect, and same in deodorize
Time can be effectively retained garlicin.
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 → immersion deodorization → 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 garlic tablet clean water after 2.2.2 being soaked.
Measure variable concentrations the most respectively, the mashed garlic weighed is extracted by the ethanol of different volumes, and extraction is certain
After time, pouring 100ml centrifuge tube centrifugal 5min under 1400rpm into, then take supernatant, filter, filtrate is the Bulbus Allii at initial stage
Element lixiviating solution.By measuring the content of contained garlicin in garlicin lixiviating solution, the most different extraction processes is for garlicin
Extraction degree, compare the garlicin extraction process drawing optimization.
Under table 1 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.
Under table 2 different condition, Bulbus Allii is carried out the impact of garlicin extraction
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 60ml 98% by 20g mashed garlic at 30 DEG C
Ethanol is the technique that extractant extracts 60min, and the extraction to garlicin is the most abundant.Meanwhile, before deodorizing method of the present invention
Under process, not interfering with Allicin Content, the deodorizing method of the present invention has preferable deodorising effect, and while deodorize
Garlicin can be effectively retained.
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. the pre-treatment deodorizing method of 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) deodorization is soaked: the garlic tablet of step (1) gained being immersed in deodorant liquid and soak 20-30h, deodorant liquid is mass percent
Fumaric acid solution for 2.5-3.5%；
(3) extraction purification: garlic tablet clean water step (2) soaked, is subsequently processed into mashed garlic, extracts the Bulbus Allii in mashed garlic
Element obtains garlicin extracting solution, is then peeled off purification, prepares pure garlicin.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 1, it is characterised in that described step
(2) deodorant liquid in is fumaric acid, acetic acid mixed solution, and in mixed solution, the mass percent of fumaric acid solution is
2.5-3.5%, the mass percent of acetic acid is 1.5-3.0%.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 1 and 2, it is characterised in that described step
Suddenly in (2), the mass percent of fumaric acid solution is 2.5-3.0%.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 3, it is characterised in that described anti-butylene
The mass percent of diacid solution is 2.8%.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 1 and 2, it is characterised in that described step
Suddenly in (2), soak time is 22-25h.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 5, it is characterised in that described step
(2) in, soak time is 24h.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 2, it is characterised in that described step
(2), in, the mass percent of acetic acid is 2.0-2.5%.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 7, it is characterised in that described step
(2), in, the mass percent of acetic acid is 2.3%.
The pre-treatment deodorizing method of garlicin extraction process the most according to claim 1, it is characterised in that described step
(3) the concretely comprising the following steps of extraction purification: selecting mass fraction 98% ethanol is extractant, and enzymolysis placed at 30 DEG C by mashed garlic
60min, takes 600ml extractant by 200g mashed garlic and extracts 60min, obtain garlicin extracting solution, takes after garlicin extracting solution is centrifugal
Clear liquid filters, and filtrate is garlicin lixiviating solution, prepares pure garlicin by isolated and purified for garlicin lixiviating solution.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849468A (en) * | 2014-03-12 | 2014-06-11 | 青海清华博众生物技术有限公司 | Garlic essential oil extraction method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849468A (en) * | 2014-03-12 | 2014-06-11 | 青海清华博众生物技术有限公司 | Garlic essential oil extraction method |
Non-Patent Citations (3)
| Title |
|---|
| 周宇等: "酶解法提取大蒜素的工艺研究", 《化工时刊》 * |
| 陈功等: "《大蒜保鲜贮藏与深加工技术》", 30 April 2003, 中国轻工业出版社 * |
| 陈华癸等: "《生物资源再利用原理与技术》", 31 August 1999, 湖北科学技术出版社 * |
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Application publication date: 20161207 |