CN103484233B - Method and device for preparing garlic oil with racemate alliin as raw materials - Google Patents
Method and device for preparing garlic oil with racemate alliin as raw materials Download PDFInfo
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- CN103484233B CN103484233B CN201310426154.2A CN201310426154A CN103484233B CN 103484233 B CN103484233 B CN 103484233B CN 201310426154 A CN201310426154 A CN 201310426154A CN 103484233 B CN103484233 B CN 103484233B
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Abstract
The invention discloses a method and device for preparing garlic oil with racemate alliin as raw materials. The method includes the following steps: (1) loading garlic, green onion, onion or allium chinensis into a reactor after the garlic, the green onion, the onion or the allium chinensis is washed, peeled and triturated, then adding an alliin solution, meanwhile, leading in air, and stirring and/or carrying out the reaction under the ultrasound condition, and (2) adding organic solvents into a reaction system after the reaction begins to carry out continuous extraction, obtaining extracted liquor, then adding edible fat and oil, water, ethyl alcohol or acetic acid into the extracted liquor, enabling the extracted liquor to be concentrated and separated in a vacuum mode at the temperature of 30-100DEG C, and obtaining the garlic oil. According to the method for preparing the garlic oil, the racemate alliin is added in the garlic, alliinase contained in the garlic is used for enabling the alliin to be converted into the garlic oil, the natural attribute of the garlic oil is kept, the yield of the garlic oil can be greatly improved, the method is simple and easy to achieve, and quite remarkable economic benefits are achieved.
Description
Technical field
The invention belongs to field of bioconversion, be specifically related to a kind of method and the device thereof that take racemate alliin as raw material and prepare Oleum Bulbus Allii.
Background technology
Oleum Bulbus Allii is the liquid mixture with important biomolecule activity, there is antibacterial, antiviral, anti-aging, anti-metal poisoning widely, cancer-resisting, the effect such as anti-oxidant, can be used for treatment infectious diseases, digestive system, oral disease, cardiovascular and cerebrovascular diseases etc.Meanwhile, Oleum Bulbus Allii is also a kind of important fodder additives, can improve the surviving rate of the food consumption of animal, feed conversion rate and animal, reduces animal disease, and can improve animal product meat etc.Be not difficult to find out, Oleum Bulbus Allii is of many uses, and market demand is very huge.
At present, the source of Oleum Bulbus Allii and preparation mainly contain two kinds of modes: first kind of way directly extracts from garlic, and extracting method comprises supercritical methanol technology, steam method, solvent method, and because extracting method is different, the yield of Oleum Bulbus Allii exists significant difference.The maximum feature of the method is the product obtained is all-natural product, shortcoming is that in garlic, the content of amounting to of Oleum Bulbus Allii only has 0.3%, thus by the restriction, particularly recent years of garlic resource, skyrocket and the production cost of Oleum Bulbus Allii climbed up and up in garlic price one tunnel.The second way is chemical synthesis, the product that this method obtains and natural garlic main body of oil basically identical, efficiency and the yield of synthesis are all very high, but because the chemical feedstocks used in chemical synthesis may be difficult to thoroughly except clean, so people can be caused unavoidably to the worry of security, the Oleum Bulbus Allii of therefore synthesis at present is mainly used as the additive of feed.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is that providing a kind of take racemate alliin as the method that Oleum Bulbus Allii prepared by raw material, this preparation method take racemate alliin as raw material, under the condition of not separation and purification allinase, garlic is joined after directly above-mentioned raw materials being made into the aqueous solution, green onion, in onion or Onion head mud, then organic solvent continuous extraction is used, water is added in extraction liquid, food oils, ethanol or acetic acid, induction garlicin decomposes, then recycling design, obtain Oleum Bulbus Allii, simple, cost is low, productive rate is high, there is the economic benefit of highly significant.
Another object of the present invention is to provide a kind of take racemate alliin as the device that Oleum Bulbus Allii prepared by raw material.
For achieving the above object, the present invention adopts following technical scheme:
Take racemate alliin as the method that Oleum Bulbus Allii prepared by raw material, comprise the following steps:
Step one, by more than one in garlic, green onion, onion or Onion head, through cleaning, peeling and loading after smashing to pieces in reactor, then add racemate alliin solution, pass into air with the flow velocity of 10 ~ 2000mL/min simultaneously, then react under stirring and/or ultrasound condition;
Step 2, reaction beginning is after 10 ~ 60 minutes, and the flow velocity with 50 ~ 1000mL/h in reaction system adds organic solvent, carries out continuous extraction, be extracted liquid while raw material reaction; By extraction liquid in 30 ~ 100 DEG C of vacuum concentration, separation, namely obtain described Oleum Bulbus Allii.
Racemate alliin of the present invention (having another name called SACS) is according to Zhang Jian, Liu Wenying; The synthesis and characterization of three kinds of main alliins in garlic, Chinese seasonings, 2011,36(9) 37-40, in method synthesis obtain.
Preferably, the racemate alliin in the solution of racemate alliin described in step one is 5:1000 ~ 5:100 with the mass ratio of garlic, green onion, onion or Onion head.
Preferably, the concentration of the solution of racemate alliin described in step one is 0.0001 ~ 0.1mol/L.
Preferably, air flow quantity described in step one with throw garlic, green onion, onion or Onion head mass values be 100 ~ 1000 (mL/min)/kg.
Preferably, described in step one, garlic, green onion, onion or Onion head are cleaned, peeling and the service temperature of smashing process to pieces be 2 ~ 35 DEG C; Stirring velocity described in step one is 100 ~ 1000r/min; Described ultrasonic frequency is 10 ~ 100kHz; Described temperature of reaction is 20 ~ 40 DEG C.
Preferably, first add the one mixing in water, food oils, acetic acid or ethanol after being extracted liquid in step 2, then extraction liquid is carried out vacuum concentration; The quality of described water, food oils, acetic acid or ethanol is 0 ~ 5 times of the racemate alliin quality in the racemate alliin solution of step one.
Preferred, the amount of described water, food oils, acetic acid or ethanol is 0.25 ~ 5 times of the racemate alliin quality in the racemate alliin solution of step one.
Preferably, organic solvent described in step 2 comprises the one in sherwood oil, Skellysolve A, normal hexane, isohexane or ethyl acetate.
After organic solvent extraction in the present invention, recyclable after cooling.Room temperature of the present invention refers to 20 ~ 35 DEG C.
Preferably, in step 2, start the time adding organic solvent, for reaction beginning is after 10 ~ 30 minutes; The flow velocity of organic solvent is 50 ~ 600mL/h.
Take racemate alliin as the device that Oleum Bulbus Allii prepared by raw material, comprise reaction system and vacuum concentration system; Described reaction system comprises the reactor of band stirring rake, and described reactor head is connected with material feeding tube and solvent feed pipe, and reactor bottom is connected with air feed pipe, and reactor top is connected with extraction phase discharge nozzle;
Described vacuum concentration system comprises extraction liquid storage tank, vaporizer, cyclonic separator, condenser, solvent tank, Oleum Bulbus Allii storage tank and valve tube; Extraction liquid storage tank, vaporizer are connected successively with cyclonic separator, and solvent tank is all connected with cyclonic separator with Oleum Bulbus Allii storage tank; Described valve tube is connected with condenser;
Described vacuum concentration system, by solvent feed pipe and extraction phase discharge nozzle, is connected with reaction system; Extraction phase discharge nozzle two ends are ligation device and extraction liquid storage tank respectively, and solvent feed pipe two ends are ligation device and solvent tank respectively.
Preferably, described extraction liquid storage tank is provided with feed-pipe.
Low for alliin content in garlic, cause the problem that the yield of extracting directly Oleum Bulbus Allii from garlic is on the low side, the present invention adopts the racemate alliin of adding synthetic in garlic, utilize itself contain in garlic and without the allinase of separation and purification, alliin is changed into Oleum Bulbus Allii.Described vacuum concentration system realizes vacuum concentration by valve tube.
The present invention and current Technical comparing, have the following advantages and beneficial effect:
1) the present invention utilizes mechanism (the i.e. solvent effect of garlicin different decomposition in different solvents, as water, there is hydrogen bond action in acetic acid and garlicin, and only there is Van der Waals force in the organic solvent of food oils or extraction and garlicin) carry out product regulation and control, by solvent effect and temperature level, change the decomposition approach of garlicin, obtain the Oleum Bulbus Allii of heterogeneity: need better nutritivity and be worth, and can tolerate relatively heavier foul smell time, use water or acetic acid can be selected to be added drop-wise in extraction liquid, then concentrated at 60 ~ 100 DEG C of temperature, can obtain main with diallyl disulphide, Diallytrisin is the product (these two kinds of material total contents account for gross weight more than 55%) of main component, otherwise, very sensitive to stink, and (be mainly used in seasoning) when biological activity is not taken notice of very much, food oils or ethanol can be selected to mix with extraction liquid, concentrate at 30 ~ 60 DEG C of temperature and can obtain 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene are the product (total amount of these two kinds of materials accounts for gross weight more than 60%) of main component.
2) instant invention overcomes the problem of allinase easy inactivation in the reaction, significantly improve the work-ing life of enzyme.From alliin to Oleum Bulbus Allii, pilot process has an important intermediate garlicin, garlicin is monomeric compound, this compound is very unstable, in the process extracted, be very easy to resolve into a series of sulfocompound, and garlicin can react with sulfydryl in allinase, causes the inactivation that allinase is too early.The method that the present invention is extracted by limit coronite, is conducive in time reaction product being shifted out system, garlicin is shifted out outside system, makes allinase have the longer life-span, prevents product from causing the inactivation of enzyme, improves the work-ing life of enzyme, improves reaction efficiency.
3) cost advantage.Alliin in a, prior art is all optical activity alliin, chemical name: (S)-3-(allyl group sulfinyl)-ALANINE, and theoretical specific rotation light value is+63.5; And the alliin raw material of the present invention is raceme, specific rotation is 0, the cost of racemate alliin greatly about natural alliin about 1/100 ~ 1/1000 (in garlic, alliin is optical activity alliin, content in garlic only 1%, and leaching process is complicated, so price is high).The present invention adopts racemate alliin to make raw material, and raw materials cost significantly lowers; B, the present invention do not need to carry out separation and purification to allinase, utilize itself contain in garlic and allinase without separation and purification carries out catalyzed conversion, alliin is changed into Oleum Bulbus Allii, a large amount of production cost can be saved.
4) security is good.The Oleum Bulbus Allii that the present invention is prepared with the racemate alliin of chemosynthesis, its composition and the Oleum Bulbus Allii directly extracted from garlic, no matter composition is basically identical (is for raw material or directly extract Oleum Bulbus Allii from garlic with racemate alliin and optical activity alliin, all utilize allinase first alliin to be changed into garlicin, garlicin instability decomposes generation Oleum Bulbus Allii), there is higher security and nutritive property; And with the Oleum Bulbus Allii of chemosynthesis in prior art because chemical feedstocks may be difficult to, thoroughly except clean, to there is food safety risk, thus at present its for feed.
Accompanying drawing explanation
Fig. 1 is the present invention take racemate alliin as the setting drawing that Oleum Bulbus Allii prepared by raw material.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
As shown in Figure 1, a kind of is the device that Oleum Bulbus Allii prepared by raw material with racemate alliin, comprises reaction system I and vacuum concentration system II; Described reaction system I comprises the reactor 7 of band stirring rake 3, and described reactor 7 top is connected with material feeding tube 1 and solvent feed pipe 6, and reactor bottom is connected with air feed pipe 2, and reactor 7 top is connected with extraction phase discharge nozzle 8;
Described vacuum concentration system II comprises extraction liquid storage tank 9, vaporizer 12, cyclonic separator 14, condenser 10, solvent tank 11, Oleum Bulbus Allii storage tank 15 and valve tube 13; Extraction liquid storage tank 9, vaporizer 12 are connected successively with cyclonic separator 14, extraction liquid in extraction liquid storage tank 9 is after vaporizer 12 vacuum concentration, enter cyclonic separator 14 separation and obtain organic solvent and Oleum Bulbus Allii, organic solvent is by entering solvent tank 11 after condenser 10 condensation, and Oleum Bulbus Allii enters Oleum Bulbus Allii storage tank 15; Described valve tube 13 is connected with condenser 10, and described vacuum concentration system II realizes vacuum concentration by valve tube 13;
Described vacuum concentration system II, by solvent feed pipe 6 and extraction phase discharge nozzle 8, is connected with reaction system I, and extraction phase discharge nozzle 8 two ends are ligation device 7 and extraction liquid storage tank 9 respectively, and solvent feed pipe 6 two ends are ligation device 7 and solvent tank 11 respectively.
Described extraction liquid storage tank 9 is provided with feed-pipe 16.
The present invention is a kind of take racemate alliin as the method that Oleum Bulbus Allii prepared by raw material, clean, peeling and the garlic after smashing to pieces, green onion, onion or Onion head raw material, reactor 7 is added from material feeding tube 1 with racemate alliin solution, pass into air from air feed pipe 2 simultaneously, under the stirring of stirring rake 3, then start reaction; Reaction beginning, after 10 ~ 60 minutes, adds organic solvent from solvent feed pipe 6 and carries out continuous extraction, be extracted liquid 4 and reacting phase 5; Extraction liquid 4 enters extraction liquid storage tank 9 from extraction phase discharge nozzle 8, then enter vaporizer 12 and carry out vacuum concentration at 30 ~ 100 DEG C, concentrated solution is separated by cyclonic separator 14 and obtains Oleum Bulbus Allii product and organic solvent, Oleum Bulbus Allii product introduction Oleum Bulbus Allii storage tank 15 is preserved, organic solvent is then reclaimed by condenser 10 condensation, and the organic solvent after recovery enters solvent tank 11 recycle.
Keep reaction carrying out in the process extracted reacting phase 5, thus achieve reaction and carry out with extraction simultaneously, enhance productivity and product purity.
Extraction liquid 4 first can drip water, food oils, acetic acid or ethanol by feed-pipe 16 and allocate, and then enters vaporizer 12 vacuum concentration.
Comparative example:
Step one, takes 1 kilogram of garlic, peeling, clean, smash to pieces at 30 DEG C after join in reactor, pump into the alliin solution 1500mL of 0.06mol/L, pass into air (flow is 300mL/min), then start Vltrasonic device, frequency is 40kHz simultaneously; Temperature of reaction 20 DEG C;
Step 2, reaction beginning, after 30 minutes, adds 1000mL ethyl acetate and at room temperature carries out continuous extraction in reaction system; Extraction liquid is vacuum concentration at 30 DEG C, is separated and after recycling design, namely obtains described Oleum Bulbus Allii 4.3 grams.
Alliin transformation efficiency is 55%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene accounts for 69.481%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene account for 11.043%, diallyl disulphide and Diallytrisin and diallyl thioether do not detect substantially.
Embodiment 1:
Step one, takes 1 kilogram of garlic, peeling, clean, smash to pieces at 30 DEG C after join in reactor, and pump into the alliin solution 1500mL of 0.06mol/L, pass into air (flow is 300mL/min), then start Vltrasonic device, frequency is 40kHz simultaneously; Temperature of reaction 20 DEG C;
Step 2, reaction beginning after 20 minutes, adding flow velocity is that the ethyl acetate of 100mL/h at room temperature carries out continuous extraction, is extracted liquid and reacting phase; Extraction liquid is vacuum concentration at 30 DEG C, and concentrated solution is separated and obtains Oleum Bulbus Allii product 7.1 grams and organic solvent.Organic solvent recycle.
Alliin transformation efficiency is 85%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene accounts for 70.40%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene account for 12.01%, diallyl disulphide and Diallytrisin and diallyl thioether do not detect substantially.
Embodiment 2:
Step one, take 1 kilogram of garlic, peeling, clean, smash to pieces at 25 DEG C after join reactor 7 from material feeding tube 1, and the racemate alliin solution 2000mL of 0.01mol/L is pumped into from material feeding tube 1, air (flow is 200mL/min) is passed into from air feed pipe 2, then start stirring rake 3, rotating speed is 100r/min; Temperature of reaction 20 DEG C;
Step 2, reaction beginning after 10 minutes, adding flow velocity from solvent feed pipe 6 is that the normal hexane of 50mL/h at room temperature carries out continuous extraction, is extracted liquid 4 and reacting phase 5; Dripping 2mL water from feed-pipe 16 makes it simply mix with extraction liquid (not exclusively mixing), extraction liquid 4 enters extraction liquid storage tank 9 from extraction phase discharge nozzle 8, then enter vaporizer 12 and at 100 DEG C vacuum concentration, concentrated solution is separated by cyclonic separator 14 and obtains Oleum Bulbus Allii product 3.9 grams and organic solvent, Oleum Bulbus Allii product introduction Oleum Bulbus Allii storage tank 15 is preserved, organic solvent is then reclaimed by condenser 10 condensation, organic solvent after recovery also, after being separated a small amount of water, enters solvent tank 11 recycle.
Alliin transformation efficiency is 93%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene accounts for 20.88%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene accounts for 2.22%, diallyl disulphide accounts for 17.34%, and Diallytrisin accounts for 40.21%, and diallyl thioether accounts for 3.11%.
Embodiment 3:
Step one, takes 1 kilogram of garlic, peeling, clean, smash to pieces at 2 DEG C after join in reactor, and pump into the racemate alliin solution 2000mL of 0.02mol/L, pass into air (flow is 500mL/min), then start stirring rake stirring reaction, rotating speed is 500r/min; Temperature of reaction 30 DEG C;
Step 2, reaction beginning after 30 minutes, adding flow velocity is that the Skellysolve A of 100mL/h at room temperature carries out continuous extraction, is extracted liquid and reacting phase; Add 3mL acetic acid to mix with extraction liquid, then by extraction liquid vacuum concentration at 60 DEG C, concentrated solution obtains Oleum Bulbus Allii product 5.6 grams and organic solvent after being separated.Organic solvent utilizes through alkali cleaning Posterior circle.
Alliin transformation efficiency is 90%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene accounts for 26.23%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene accounts for 3.22%, diallyl disulphide accounts for 18.34%, and Diallytrisin accounts for 37.22%, and diallyl thioether accounts for 2.01%.
Embodiment 4:
Step one, takes 1 kilogram of garlic, peeling, clean, smash to pieces at 10 DEG C after join in reactor, and pump into the racemate alliin solution 1000mL of 0.1mol/L, pass into air (flow is 1000mL/min), then start stirring rake stirring reaction, rotating speed is 1000r/min; Temperature of reaction 40 DEG C;
Step 2, reaction beginning after 30 minutes, adding flow velocity is that the isohexane of 100mL/h at room temperature carries out continuous extraction, is extracted liquid and reacting phase; Add 5mL food oils to mix with extraction liquid, then by extraction liquid vacuum concentration at 50 DEG C, concentrated solution obtains Oleum Bulbus Allii product 6.5 grams and organic solvent after being separated.Organic solvent recycle and reuse.
Alliin transformation efficiency is 65%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene and accounts for 14.45%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene accounts for 49.31%,, Diallytrisin accounts for 2.97%, and diallyl thioether and diallyl disulphide do not detect.
Embodiment 5:
Step one, takes 1 kilogram of Onion head, peeling, clean, smash to pieces at 35 DEG C after join in reactor 7, and pump into the alliin solution 1400mL of 0.10mol/L, pass into air (flow is 500mL/min), then start Vltrasonic device, frequency is 100kHz simultaneously; Temperature of reaction 40 DEG C;
Step 2, reaction beginning after 60 minutes, adding flow velocity is that the sherwood oil of 1000mL/h at room temperature carries out continuous extraction, is extracted liquid and reacting phase; Drip 10mL ethanol to mix with extraction liquid, then by extraction liquid vacuum concentration at 40 DEG C, concentrated solution obtains Oleum Bulbus Allii product 5.2 grams and organic solvent after being separated.Organic solvent recycle and reuse.
Alliin transformation efficiency is 56%.Adopt gas chromatographic detection, Oleum Bulbus Allii consists of 3-vinyl-1,2-bis-sulphur hexamethylene-5-alkene and accounts for 44.45%(percentage contents) and 3-vinyl-1,2-bis-sulphur hexamethylene-4-alkene accounts for 28.31%,, Diallytrisin accounts for 5.77%, and diallyl thioether and diallyl disulphide do not detect.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. be the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, comprise the following steps:
Step one, by more than one in garlic, green onion, onion or Onion head, through cleaning, peeling and loading after smashing to pieces in reactor, then add racemate alliin solution, pass into air with the flow velocity of 10 ~ 2000mL/min simultaneously, then react under stirring and/or ultrasound condition;
Step 2, reaction beginning is after 10 ~ 60 minutes, and the flow velocity with 50 ~ 1000mL/h in reaction system adds organic solvent, carries out continuous extraction, be extracted liquid while raw material reaction; By extraction liquid in 30 ~ 100 DEG C of vacuum concentration, separation, namely obtain described Oleum Bulbus Allii.
2. according to claim 1 take racemate alliin as the method that Oleum Bulbus Allii prepared by raw material, it is characterized in that, racemate alliin in the solution of racemate alliin described in step one is 1:100 ~ 5:100 with the mass ratio of garlic, green onion, onion or Onion head.
3. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, the concentration of the solution of racemate alliin described in step one is 0.0001 ~ 0.1mol/L.
4. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, air flow quantity described in step one with throw garlic, green onion, onion or Onion head mass values be 100 ~ 1000 (mL/min)/kg.
5. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, by garlic, green onion, onion or Onion head described in step one, cleans, peeling and the service temperature of smashing process to pieces be 2 ~ 35 DEG C; Stirring velocity described in step one is 100 ~ 1000r/min; Described ultrasonic frequency is 10 ~ 100kHz; Described temperature of reaction is 20 ~ 40 DEG C.
6. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, and it is characterized in that, organic solvent described in step 2 comprises the one in sherwood oil, Skellysolve A, normal hexane, isohexane or ethyl acetate.
7. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, first adds the one mixing in water, food oils, acetic acid or ethanol, then extraction liquid is carried out vacuum concentration in step 2 after being extracted liquid; The quality of described water, food oils, acetic acid or ethanol is 0.25 ~ 5 times of the racemate alliin quality in the racemate alliin solution of step one.
8. according to claim 1 is the method that Oleum Bulbus Allii prepared by raw material with racemate alliin, it is characterized in that, starts the time adding organic solvent in step 2, for reaction beginning is after 10 ~ 30 minutes; The flow velocity of organic solvent is 50 ~ 600mL/h.
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| CN104087627A (en) * | 2014-07-29 | 2014-10-08 | 江南大学 | Method for preparing gram-level high-purity natural thiosulfinate |
| CN108254460B (en) * | 2017-12-28 | 2020-05-12 | 云南农业大学 | Method for detecting thioether compounds in garlic root exudates |
| CN111796036B (en) * | 2020-07-07 | 2023-03-17 | 清远市食品检验中心 | Detection method for identifying natural garlic oil adulterated with synthetic garlic oil |
| CN114703239B (en) * | 2022-03-22 | 2022-09-30 | 辰欣药业股份有限公司 | Production method of allicin |
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