CN108342421A - A kind of allicin extracting method - Google Patents

A kind of allicin extracting method Download PDF

Info

Publication number
CN108342421A
CN108342421A CN201810142861.1A CN201810142861A CN108342421A CN 108342421 A CN108342421 A CN 108342421A CN 201810142861 A CN201810142861 A CN 201810142861A CN 108342421 A CN108342421 A CN 108342421A
Authority
CN
China
Prior art keywords
allicin
garlic
filtrate
extracting method
enzyme
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810142861.1A
Other languages
Chinese (zh)
Inventor
余赞
张礼
钟文
张孝龙
田璐
罗辉
文彪
罗臻
钱正宇
杜建军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changde Jinde New Material Technology Co Ltd
Original Assignee
Changde Jinde New Material Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changde Jinde New Material Technology Co Ltd filed Critical Changde Jinde New Material Technology Co Ltd
Priority to CN201810142861.1A priority Critical patent/CN108342421A/en
Publication of CN108342421A publication Critical patent/CN108342421A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P11/00Preparation of sulfur-containing organic compounds

Landscapes

  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Preparation Of Fruits And Vegetables (AREA)

Abstract

This application discloses a kind of allicin extracting methods, it is therefore intended that, keep technical process simple, easy to operation, cost is relatively low, without other bad smells and dissolvent residual, improves the recovery rate of allicin, used technical solution is:Include the following steps:1) garlic is smashed to pieces as mashed garlic;2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs;3) by mashed garlic, constant temperature digests at a temperature of 30 80 DEG C, obtains enzymolysis liquid;4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, filtrate is merged;5) soxhlet extraction several times carried out to the filtrate after merging using ethyl alcohol, the solid-liquid ratio of filtrate and ethyl alcohol is (1:4)‑(1:14) g/mL obtains extract liquor;6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;7) allicin solution is concentrated under reduced pressure to get to allicin using Rotary Evaporators.

Description

A kind of allicin extracting method
Technical field
This application involves technical field of plant extraction, and in particular to a kind of allicin extracting method.
Background technology
Allicin is three thio-allyl ether class compounds, is pale yellow powder or pale yellow oily liquid, generally has denseer Smell.80-85 DEG C of boiling point (0.2kPa), relative density 1.112 (20/4 DEG C), index of refraction 1.561.Be dissolved in ethyl alcohol, chloroform or Ether.Solubility 2.5% (quality) (10 DEG C) in water, pH value of water solution 6.5, when standing, have oil deposit to be formed. With ethyl alcohol, ether and benzene can dissolve each other.It is unstable to thermokalite, acid is stablized.By being present in the bulb of liliaceous plant garlic, by Existing garlic aminoacid converts generation under that action of alliinase.It exists in the bulb of green onion, there is strong big garlic odour, taste It is peppery.Allicin is naturally occurring in the bulb of liliaceous plant garlic.There is antibacterial work to a variety of Gram-positives and negative bacterium With to bacillus (shigella dysenteriae, typhoid bacillus, Escherichia coli, Bordetella pertussis), fungi, (Candida albicans, cryptococcus, cigarette are bent Mould), viral (cytomegalovirus), Amoeba, Trichomonas vaginalis, pinworm etc. have inhibition killing effect, especially to large intestine The effect of the enteric bacteria such as bacillus, shigella dysenteriae is strong.
There are mainly three types of the extracting methods of existing allicin:Steam distillation, organic solvent extraction and overcritical Extraction, equipment needed for steam distillation is simple, and technique is relatively simple, easy to operate, but the recovery rate of allicin compares It is low;Organic solvent extraction is extracted using organic solvent, can residual organic solvent in allicin;Although supercritical extraction Recovery rate is high, quality is preferable, but production cost is higher, and equipment is complex, and the technical difficulty of operation is larger.Therefore it needs to open It is relatively low to send out cost a kind of, simple for process, but the higher method of recovery rate of allicin.
Invention content
In order to solve the problems in the prior art, easy to operation present applicant proposes a kind of technical process is simple, cost compared with It is low, be free of other bad smells and dissolvent residual, and the higher allicin extracting method of recovery rate of allicin.
In order to achieve the goal above, technical solution used by the application is:Include the following steps:
1) garlic is smashed to pieces as mashed garlic;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 5-7 to make the pH of mixed liquor;
3) so that constant temperature at a temperature of 30-80 DEG C is digested 30-150min, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 1-6h, filtrate and ethyl alcohol are carried out to the filtrate after merging using ethyl alcohol Solid-liquid ratio be (1:4)-(1:14) g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 50- 150r/s, vapo(u)rizing temperature are 30-80 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
It uses tissue mashing machine to smash garlic for mashed garlic to pieces in the step 1), garlic is cleaned and dripped before smashing to pieces It is dry.
Catalyzing enzyme is at least one of allinnase, cellulase, hemicellulase and pectase in the step 2).
In the step 2) in mixed liquor catalyzing enzyme a concentration of 120-180U/L.
Enzymolysis catalyst is also added in the step 2) into mashed garlic.
The enzymolysis catalyst is Fe2+Ion, Cu2+Ion and Mn2+One kind in ion, it is described to digest the dense of catalyst Degree is 6-12mmol/L.
The pH buffer solutions are one kind in phosphate buffer and citrate buffer.
Mashed garlic is digested into 50-70min in 40-50 DEG C of thermostat water bath in the step 3).
Ethyl alcohol is 95% ethyl alcohol in the step 5), and the solid-liquid ratio of preferred filtrate and ethyl alcohol is in soxhlet extraction:1: 10g/mL, extraction time 3-4h.
The rotating speed of preferred Rotary Evaporators is 90-110r/s in the step 7), and vapo(u)rizing temperature is 40-50 DEG C.
Compared with prior art, the application smashs garlic to pieces to add catalyzing enzyme after mashed garlic and adjusting pH, makes mixed liquor PH is 5-7, and suitable acid or alkali environment is conducive to keep the activity of catalyzing enzyme, and combines suitable hydrolysis temperature and time, makes to urge Changing enzyme can make the alliin in mashed garlic be sufficiently converted into allicin, and repeat progress several times to digesting filtered filter residue Enzymolysis and filtering, can be such that remaining alliin in filter residue is adequately converted, and rope several times is carried out to filtrate using ethyl alcohol Family name extracts, and improves the recovery rate of allicin, carries out soxhlet extraction furthermore with ethyl alcohol, ethyl alcohol is volatile and to human body side effect It is small, since boiling point significant difference is easily isolated after extraction, without other bad smells and dissolvent residual, using carrying for the application Method is taken, technical process is simple, easy to operation, and cost is relatively low, and the recovery rate of allicin is higher.
Further, catalyzing enzyme is added in mashed garlic, catalyzing enzyme is allinnase, cellulase, hemicellulase or pectin Enzyme, allinnase can promote the conversion of alliin, pectase that the intercellular damage layer of plant cell, cell can be made to detach, to So that cortex is fallen off, be added in fruit smashing object, fruit juice can not only be made to be easy to squeeze, and crushing juice rate can also be improved.Cellulose Enzyme can destroy cell wall, release intracellular matter, be a kind of enzyme preparation for starch and alcohol industry, can reduce viscosity With improvement and the separation of different cereal crops.The enzyme preparation of cellulase can be improved effectively and digest plant cell structures Non-starch carbohydrate.Promoted using cellulase or hemicellulase or pectase in the application intercellular in garlic It destroys, more promotes enzymolysis.
Further, due to Fe2+、Cu2+、Mn2+Certain activation is all had to cellulase and allinnase, it can be with Zymoexciter and cellulase collocation are used, is digested with further promotion, improves the recovery rate of allicin.
Specific implementation mode
The application is further explained with reference to specific embodiment.
The application first smashs garlic for mashed garlic to pieces, addition catalyzing enzyme, enzymolysis catalyst and pH buffer solutions into mashed garlic, and Constant temperature digests in thermostat water bath;It is filtered after enzymolysis, ethyl alcohol soxhlet extraction is carried out to filtrate, obtains allicin solution, Finally allicin solution is centrifuged and is concentrated under reduced pressure successively purification to get to allicin, the application utilizes catalyzing enzyme Alliin is promoted to be converted into allicin, catalyzing enzyme is allinnase, cellulase, hemicellulase or pectase, enzymolysis catalysis Agent is Fe2+Ion, Cu2+Ion or Mn2+Ion is substantially increased the conversion ratio of enzymolysis using catalyzing enzyme and enzymolysis catalyst, carried The high output capacity of allicin.
Important physiological activity substance, allinnase also known as alliin lyase or half Guangs of S- alkyl-L- on allinnase Propylhomoserin sulfoxide enzyme, is present in the plants such as garlic, onion, leek, is containing there are two the dimer glycoprotein of same subunit, garlic ammonia Sour enzyme, which is contacted and is catalyzed with alliin, generates the allicin with valuable pharmacological purposes.
Cellulase is the general name of the glucogenic one group of enzyme of degraded cellulose, its not instead of monomeric enzyme plays collaboration The multicomponent enzyme system of effect is a kind of complex enzyme, mainly by circumscribed 1,4 beta-glucanase, Endo-β-glucanase and beta-glucosidase The compositions such as enzyme, the zytase of also very high vigor.The product for acting on cellulose and being derived from cellulose.Microorganism Cellulase destroys cell wall to improve fruit juice yield etc. in conversion insoluble fibrin at glucose and in juice Aspect has very important significance.Cellulase can destroy cell wall, release intracellular matter, be it is a kind of for starch and The enzyme preparation of alcohol industry can reduce viscosity and improve and the separation of different cereal crops.The enzyme preparation of cellulase can be with It is non-starch carbohydrate effectively to improve and digest plant cell structures.
Hemicellulase is a kind of enzyme that the polysaccharide of composition plant cell membrane can be made to hydrolyze, and can promote plant cell wall Dissolving, so that more plant cell Dissolve things insides is dissolved out, and by stodgy macromolecular polysaccharide, protein and lipid drop Solution is small-molecule substance, has facilitation to the enzymolysis of garlic.
Pectase refers to the enzyme for decomposing plant main component-pectic substance.Pectase is distributed widely in higher plant and micro- In biology, pectase is most important enzyme in fruit process, and fruit is crushed using pectinase treatment, fruit juice can be accelerated to filter, and is promoted Into clarification etc., pectase can make the intercellular damage layer of plant cell, cell separation that it is broken to be added to fruit to make cortex fall off In mincing, fruit juice can not only be made to be easy to squeeze, and crushing juice rate can also be improved.
Enzymolysis catalyst can change an inactive enzyme precursor (proenzyme), make active enzyme, or accelerate certain The rate of kind enzyme reaction generates activation of enzymes.Various metals ion, especially Fe2+Ion, Cu2+Ion or Mn2+Ion etc. is The activator of certain enzymes, they serve as a connection when enzyme-to-substrate combines, the catalytic action of kinase.
Phosphate buffer uses the buffer solution that sodium dihydrogen phosphate and disodium hydrogen phosphate are made into, citric acid in the present embodiment Salt buffer uses citric acid-sodium citrate buffer.The pH conditions of enzymolysis are to be adjusted to pH value using buffer solution to exist Between 5-7, in favor of the activity of catalyzing enzyme.
Embodiment 1:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 6 to make the pH of mixed liquor, and catalyzing enzyme is allinnase And cellulase, a concentration of 120U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst is also added in mashed garlic, enzymolysis catalyst is Fe2+Solion digests a concentration of 6mmol/L of catalyst;PH buffer solutions are phosphate buffer;
3) make mashed garlic at a temperature of 40 DEG C that constant temperature digests 50min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 4h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:10g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 100r/ S, vapo(u)rizing temperature are 45 DEG C, and pressure is 0.01Mpa to get to allicin.
Embodiment 2:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 5 to make the pH of mixed liquor, and catalyzing enzyme is alliin Enzyme, hemicellulase and pectase, a concentration of 140U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst is also added in mashed garlic, Enzymolysis catalyst is Cu2+Ion digests a concentration of 8mmol/L of catalyst;PH buffer solutions are citrate buffer;
3) make mashed garlic at a temperature of 45 DEG C that constant temperature digests 45min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 3h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:4g/mL obtains extract liquor;Ethyl alcohol is ethyl alcohol;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution being concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 90r/s, Vapo(u)rizing temperature is 40 DEG C, and pressure is 0.02Mpa to get to allicin.
Embodiment 3:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 7 to make the pH of mixed liquor, and catalyzing enzyme is alliin Enzyme, cellulase, hemicellulase and pectase, a concentration of 180U/L of catalyzing enzyme in mixed liquor;Enzyme is also added in mashed garlic Catalyst is solved, enzymolysis catalyst is Mn2+Ion digests a concentration of 10mmol/L of catalyst;PH buffer solutions are phosphate-buffered Liquid;
3) make mashed garlic at a temperature of 50 DEG C that constant temperature digests 40min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 5h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:8g/mL obtains extract liquor;Ethyl alcohol is ethyl alcohol;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 110r/ S, vapo(u)rizing temperature are 50 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
Embodiment 4:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 6.5 to make the pH of mixed liquor, and catalyzing enzyme is alliin Enzyme, a concentration of 160U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst is also added in mashed garlic, enzymolysis catalyst is Cu2+Ion, Digest a concentration of 12mmol/L of catalyst;PH buffer solutions are citrate buffer;
3) make mashed garlic at a temperature of 80 DEG C that constant temperature digests 30min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 6h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:6g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 150r/ S, vapo(u)rizing temperature are 30 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
Embodiment 5:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 5.5 to make the pH of mixed liquor, and catalyzing enzyme is cellulose Enzyme and hemicellulase, a concentration of 130U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst, enzymolysis catalysis are also added in mashed garlic Agent is Fe2+Ion digests a concentration of 10mmol/L of catalyst;PH buffer solutions are phosphate buffer;
3) make mashed garlic at a temperature of 30 DEG C that constant temperature digests 150min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 3h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:12g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 130r/ S, vapo(u)rizing temperature are 60 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
Embodiment 6:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 5.8 to make the pH of mixed liquor, and catalyzing enzyme is alliin Enzyme and pectase, a concentration of 150U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst is also added in mashed garlic, enzymolysis catalyst is Mn2+Ion digests a concentration of 10mmol/L of catalyst;PH buffer solutions are citrate buffer;
3) make mashed garlic at a temperature of 60 DEG C that constant temperature digests 50min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 2h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:14g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 50, is steamed It is 70 DEG C to evaporate temperature, and pressure is 0.01-0.02Mpa to get to allicin.
Embodiment 7:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 7 to make the pH of mixed liquor, and catalyzing enzyme is cellulase And pectase, a concentration of 170U/L of catalyzing enzyme in mixed liquor;Enzymolysis catalyst is also added in mashed garlic, enzymolysis catalyst is Cu2+Ion digests a concentration of 7mmol/L of catalyst;PH buffer solutions are citrate buffer;
3) make mashed garlic at a temperature of 70 DEG C that constant temperature digests 40min in thermostat water bath, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times, extraction time 1h, filtrate and second are carried out to the filtrate after merging using 95% ethyl alcohol The solid-liquid ratio of alcohol is 1:13g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution being concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 80r/s, Vapo(u)rizing temperature is 60 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
Embodiment 8:
The present embodiment specifically includes following steps:
1) it chooses free from insect pests, without the high-quality garlic to go mouldy, garlic is cleaned and dripped with clear water after carrying out point valve peeling It is dry, use tissue mashing machine to smash garlic for mashed garlic to pieces;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 6.7 to make the pH of mixed liquor, and catalyzing enzyme is hemicellulose Plain enzyme and pectase, a concentration of 145U/L of catalyzing enzyme in mixed liquor;It is also added with enzymolysis catalyst in mashed garlic, digests catalyst For Mn2+Ion digests a concentration of 9mmol/L of catalyst;PH buffer solutions are phosphate buffer;
3) make mashed garlic at a temperature of 65 DEG C that constant temperature digests 120min in thermostat water bath;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, by filtrate Merge;
5) soxhlet extraction several times carried out to the filtrate after merging using 95% ethyl alcohol, extraction time 1-6h, filtrate and The solid-liquid ratio of ethyl alcohol is 1:9g/mL obtains extract liquor;Ethyl alcohol is ethyl alcohol;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution is concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 120r/ S, vapo(u)rizing temperature are 70 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
By a large number of experiments verification and product analysis, the preferred catalyzing enzyme scheme of the application is that allinnase adds cellulose It is one or more in enzyme, hemicellulase and pectase, preferred 40-50 DEG C of the temperature of enzymolysis, time 50-70min;Soxhlet The solid-liquid ratio of preferred filtrate and ethyl alcohol is in extraction:1:10g/mL, extraction time 3-4h;Preferred Rotary Evaporators turn Speed is 90-110r/s, and vapo(u)rizing temperature is 40-50 DEG C, and higher recovery rate can be obtained using preferred technological parameter.
The application smashs garlic to pieces to add catalyzing enzyme and zymoexciter after mashed garlic, and catalyzing enzyme, catalyzing enzyme is added in mashed garlic For allinnase, cellulase, hemicellulase or pectase, allinnase can promote the conversion of alliin, pectase energy The intercellular damage layer of plant cell, cell separation is set to make cortex fall off, to be added in fruit smashing object, fruit can not only be made Juice is easy to squeeze, and can also improve crushing juice rate.Cellulase can destroy cell wall, release intracellular matter, be a kind of use In the enzyme preparation of starch and alcohol industry, viscosity can be reduced and improved and the separation of different cereal crops.The enzyme of cellulase It is non-starch carbohydrate that plant cell structures can effectively be improved and be digested to preparation.In the application using cellulase or Hemicellulase or pectase promote intercellular destruction in garlic, more promote enzymolysis.Due to Fe2+、Cu2+、Mn2+To fiber Plain enzyme all has certain activation with allinnase, can use zymoexciter and cellulase collocation, with further Promotion enzymolysis, improve the recovery rate of allicin.
The application adjusts the pH of enzymolysis using phosphate buffer and citrate buffer as pH buffer solutions, suitably Acid or alkali environment is conducive to keep the activity of catalyzing enzyme, and combines suitable hydrolysis temperature and time, and catalyzing enzyme is enable to make mashed garlic In alliin be sufficiently converted into allicin, and repeat progress to digesting filtered filter residue and digest and filter, energy several times So that remaining alliin in filter residue is adequately converted, soxhlet extraction several times is carried out to filtrate using ethyl alcohol, is improved The recovery rate of allicin, furthermore with ethyl alcohol carry out soxhlet extraction, ethyl alcohol is volatile and to human body Small side effects, after extraction due to Boiling point significant difference is easily isolated, without other bad smells and dissolvent residual.Using the extracting method of the application, technique mistake Journey is simple, easy to operation, and cost is relatively low, and the recovery rate of allicin is higher.
The above is only the specific implementation mode of the application, is made skilled artisans appreciate that or realizing this Shen Please.Various modifications to these embodiments will be apparent to one skilled in the art, as defined herein General Principle can in other embodiments be realized in the case where not departing from spirit herein or range.Therefore, the application It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest range caused.
It should be understood that the application is not limited to the content being described above out, and it can not departed from Range carry out various modifications and changes.Scope of the present application is only limited by the accompanying claims.

Claims (10)

1. a kind of allicin extracting method, which is characterized in that include the following steps:
1) garlic is smashed to pieces as mashed garlic;
2) catalyzing enzyme and pH buffer solutions are added into mashed garlic and stirs, it is 5-7 to make the pH of mixed liquor;
3) so that constant temperature at a temperature of 30-80 DEG C is digested 30-150min, obtain enzymolysis liquid;
4) enzymolysis liquid is filtered, obtains filtrate and filter residue;And filter residue is repeated to digest and is filtered several times, filtrate is closed And;
5) soxhlet extraction several times, extraction time 1-6h, the material of filtrate and ethyl alcohol are carried out to the filtrate after merging using ethyl alcohol Liquor ratio is (1:4)-(1:14) g/mL obtains extract liquor;
6) extract liquor is put into centrifuge and is centrifuged, obtain allicin solution;
7) allicin solution being concentrated under reduced pressure using Rotary Evaporators, the rotating speed for controlling Rotary Evaporators is 50-150r/s, Vapo(u)rizing temperature is 30-80 DEG C, and pressure is 0.01-0.02Mpa to get to allicin.
2. a kind of allicin extracting method according to claim 1, which is characterized in that smash using tissue in the step 1) Broken machine smashs garlic for mashed garlic to pieces, and garlic is cleaned and drained before smashing to pieces.
3. a kind of allicin extracting method according to claim 1, which is characterized in that catalyzing enzyme is garlic in the step 2) At least one of propylhomoserin enzyme, cellulase, hemicellulase and pectase.
4. a kind of allicin extracting method according to claim 3, which is characterized in that urged in mixed liquor in the step 2) Change a concentration of 120-180U/L of enzyme.
5. a kind of allicin extracting method according to claim 1, which is characterized in that in the step 2) also into mashed garlic Added with enzymolysis catalyst.
6. a kind of allicin extracting method according to claim 5, which is characterized in that the enzymolysis catalyst is Fe2+From Son, Cu2+Ion and Mn2+One kind in ion, a concentration of 6-12mmol/L of the enzymolysis catalyst.
7. according to a kind of allicin extracting method of claim 1-6 any one of them, which is characterized in that the pH buffer solutions are One kind in phosphate buffer and citrate buffer.
8. according to a kind of allicin extracting method of claim 1-6 any one of them, which is characterized in that will in the step 3) Mashed garlic digests 50-70min in 40-50 DEG C of thermostat water bath.
9. according to a kind of allicin extracting method of claim 1-6 any one of them, which is characterized in that second in the step 5) Alcohol is 95% ethyl alcohol, and the solid-liquid ratio of preferred filtrate and ethyl alcohol is in soxhlet extraction:1:10g/mL, extraction time 3-4h.
10. according to a kind of allicin extracting method of claim 1-6 any one of them, which is characterized in that in the step 7) The rotating speed of preferred Rotary Evaporators is 90-110r/s, and vapo(u)rizing temperature is 40-50 DEG C.
CN201810142861.1A 2018-02-11 2018-02-11 A kind of allicin extracting method Pending CN108342421A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810142861.1A CN108342421A (en) 2018-02-11 2018-02-11 A kind of allicin extracting method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810142861.1A CN108342421A (en) 2018-02-11 2018-02-11 A kind of allicin extracting method

Publications (1)

Publication Number Publication Date
CN108342421A true CN108342421A (en) 2018-07-31

Family

ID=62960331

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810142861.1A Pending CN108342421A (en) 2018-02-11 2018-02-11 A kind of allicin extracting method

Country Status (1)

Country Link
CN (1) CN108342421A (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109609272A (en) * 2018-11-23 2019-04-12 盐城工学院 A kind of extracting method for the galic essential oil reducing cholesterol micella solubility
CN110215422A (en) * 2019-05-28 2019-09-10 青春妆园生物科技(广州)有限公司 A kind of allicin shines new flesh water of face moisturizing and preparation method thereof
CN110215409A (en) * 2019-05-28 2019-09-10 沈衡平 A kind of allicin moisturizing is releived maintenance water and preparation method thereof
CN110314124A (en) * 2019-07-04 2019-10-11 沈衡平 A kind of allicin moisturizing essence aqueous and preparation method thereof
CN110354016A (en) * 2019-07-04 2019-10-22 沈衡平 A kind of bright fair-skinned light sensation essence aqueous of allicin and preparation method thereof
CN110354015A (en) * 2019-07-04 2019-10-22 沈衡平 A kind of allicin drives face maintenance essence aqueous and preparation method thereof
CN111705091A (en) * 2020-07-02 2020-09-25 成都市三禾田生物技术有限公司 Preparation method of sulforaphane extract
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 (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005089419A (en) * 2003-09-19 2005-04-07 Noevir Co Ltd Garlic extract
CN103614230A (en) * 2013-11-20 2014-03-05 徐州黎明食品有限公司 Preparation method of garlic oil
CN106337070A (en) * 2016-08-24 2017-01-18 徐金蝶 Garlicin extraction method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005089419A (en) * 2003-09-19 2005-04-07 Noevir Co Ltd Garlic extract
CN103614230A (en) * 2013-11-20 2014-03-05 徐州黎明食品有限公司 Preparation method of garlic oil
CN106337070A (en) * 2016-08-24 2017-01-18 徐金蝶 Garlicin extraction method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
J. M. DEL VALLE,ET AL.: "EXTRACTION OF GARLIC WITH SUPERCRITICAL CO2 AND CONVENTIONAL ORGANIC SOLVENTS", 《BRAZILIAN JOURNAL OF CHEMICAL ENGINEERING》 *
陈超等: "外源纤维素酶对蒜素得率的影响", 《食品研究与开发》 *
黎源倩: "《中华医学百科全书卫生检验学》", 30 June 2017, 中国协和医科大学出版 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109609272A (en) * 2018-11-23 2019-04-12 盐城工学院 A kind of extracting method for the galic essential oil reducing cholesterol micella solubility
CN110215422A (en) * 2019-05-28 2019-09-10 青春妆园生物科技(广州)有限公司 A kind of allicin shines new flesh water of face moisturizing and preparation method thereof
CN110215409A (en) * 2019-05-28 2019-09-10 沈衡平 A kind of allicin moisturizing is releived maintenance water and preparation method thereof
CN110314124A (en) * 2019-07-04 2019-10-11 沈衡平 A kind of allicin moisturizing essence aqueous and preparation method thereof
CN110354016A (en) * 2019-07-04 2019-10-22 沈衡平 A kind of bright fair-skinned light sensation essence aqueous of allicin and preparation method thereof
CN110354015A (en) * 2019-07-04 2019-10-22 沈衡平 A kind of allicin drives face maintenance essence aqueous and preparation method thereof
CN111705091A (en) * 2020-07-02 2020-09-25 成都市三禾田生物技术有限公司 Preparation method of sulforaphane extract
CN111705091B (en) * 2020-07-02 2023-11-10 成都市三禾田生物技术有限公司 Preparation method of sulforaphane extract
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

Similar Documents

Publication Publication Date Title
CN108342421A (en) A kind of allicin extracting method
CN103614230B (en) Preparation method of garlic oil
CN104757564B (en) A kind of method utilizing Pericarppium arachidis hypogaeae to prepare dietary fiber
CN105341952A (en) Method for extracting soluble dietary fibers from rice bran through extruding-expansion assisted with enzymolysis
CN110272506A (en) A kind of extracting method of Fuscoporia obliqua polysaccharide
CN101891839B (en) Method for extracting and separating pectin from apple pomace
CN106349405A (en) Method for extracting pectin from shaddock peel through enzymolysis and ultrasonic waves
CN108948227A (en) A kind of method that high-voltage pulse extracts okra pectin
CN108794651A (en) The method that pectin is extracted in passion fruit pericarp
CN102911277B (en) Supercritical CO 2to extract in raffinate and the method for purified garlic polysaccharide and garlic polysaccharide are preparing the application in Yoghourt
CN107115367B (en) Fermentation production method for efficiently extracting flavone from ginkgo leaves
CN101455291B (en) Fructose and oligo-fructose production method using garlic fructosan hydrolase
CN111705091B (en) Preparation method of sulforaphane extract
CN111150069A (en) Method for preparing asparagus byproduct dietary fiber by adopting enzymolysis method and spray drying
CN104844551B (en) Method for simultaneously separating and extracting lotus flavones and polysaccharide
CN114262721A (en) Fermentation process of ginger extract, fermentation product and application thereof
CN107821924A (en) A kind of extraction process of garnet pigment
CN106811303B (en) Method for simultaneously extracting essential oil and pectin from ginkgo biloba sarcotesta
CN108300561A (en) A kind of method of aqueous enzymatic extraction peony seed oil
CN106810619B (en) A kind of gingko episperm pectin and polypentenol extracting method
CN106636039A (en) Extraction method for bromelain
CN106883314A (en) A kind of method that pectin is extracted in the slag from lemon peel
CN105433394A (en) Preparation method of pineapple residue soluble dietary fiber
CN106820170A (en) A kind of preparation method of kiwifruit peel soluble dietary fiber
CN107319577A (en) The extracting method of soluble dietary fiber in a kind of burdock

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20180731