CN101985578B - Method for improving garlic oil yield - Google Patents
Method for improving garlic oil yield Download PDFInfo
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- CN101985578B CN101985578B CN 201010526722 CN201010526722A CN101985578B CN 101985578 B CN101985578 B CN 101985578B CN 201010526722 CN201010526722 CN 201010526722 CN 201010526722 A CN201010526722 A CN 201010526722A CN 101985578 B CN101985578 B CN 101985578B
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Abstract
The invention discloses a method for improving garlic oil yield, which comprises: soaking fresh garlic or dry garlic slices in water; stirring for removing impurities such as soil; feeding the fresh garlic or dry garlic slices in a pulping machine and crushing; adding an allinase activity regulator; performing enzymolysis; adding a transforming agent; feeding; distilling; feeding distillate into distilling equipment; taking an oil phase out, wherein the oil phase is coarse garlic oil; drying the garlic oil by a silicagel column; and removing residual moisture and obtaining the garlic oil. The method has the main advantages that: when the proper transforming agent is added, the distillation time is reduced by 20 percent, the garlic oil yield is improved to 1 to 3 times, and the content of each of the components such as diallyl disulfide, diallyl trisulfide, diallyl sulfide, allyl methyl sulfide, allyl methyl disulphide, allyl methyl trisulphide, propenethiol and methyl merecaptan is improved to over 3 times; and equipment investment is not increased, as only a proper amount transforming agent is added on the basis of the original distillation garlic oil production line.
Description
Technical field
The invention belongs to deep processing of farm products, relate to and utilize garlic fresh or dehydration to produce and improve the method for garlic oil yield.
Background technology
Bulbus Allii quintessence oil has very high medicinal, edible and seasoning and is worth, and is described as " plant gold ".Studies show that: Bulbus Allii quintessence oil can kill many pathogenic bacterium such as influenza virus, staphylococcus, suis, meningococcus, typhoid fever, paratyphoid, dysentery bacterium and cholera, diphtheria, chew 5 minutes in the mouth if garlic clove is placed on, just can kill various bacteriums hiding in the oral cavity, therefore, people claim that Bulbus Allii quintessence oil is plant penicillin, vegetalitas Broad spectrum antibiotics.Modern medicine study card confirms: garlic has antitumor, anti-platelet aggregation, lipidemia and the effect of congee shape arteriosclerosis, and fortifying fibre protein dissolution active function is arranged, and vasodilation and hypotensive effect are arranged.At present, people have utilized Bulbus Allii quintessence oil to develop the Oleum Bulbus Allii injection liquid, Oleum Bulbus Allii solution, garlic emulsion, capsule with garlic refined oil, the allicin health-care skin liquid, allicin hair care, hair lotion, the allicin antistaling and antiseptic agent, etc. (Yue Tianli etc., 2003).Therefore, these effects all have direct or indirect relation with Bulbus Allii quintessence oil or Related Component.Bulbus Allii quintessence oil has become a kind of important food, medicine and cosmetic material, and along with the raising of health of people level of consciousness, the requirement of Bulbus Allii quintessence oil is with increasing.
Bulbus Allii quintessence oil is that alliin contained in the garlic generates garlicin (such as equation 1), again warp under the effect of allinase
Alliin garlicin pyruvic acid
Equation 1 forms the reaction of garlicin
The operations such as distillation, cooling, oily water separation are produced.In extracting sepn process, the mixture of more than the 30 kind of organosulfurs such as the as easy as rolling off a log formation diallyl disulfide of the garlicin that produces, garlicin, allyl methyl disulfide, diallyl thioether, allyl methyl thioether, allyl methyl trisulfide, allyl sulfhydrate, methyl mercaptan, they have consisted of Bulbus Allii quintessence oil jointly.
The method of producing Bulbus Allii quintessence oil has steam distillation (CN 200310117624.3), solvent extraction method (CN200810016047.1 etc.), supercritical co (such as CN 200810195818.8) extraction method and molecular distillation method (CN200810023771.7), rear three kinds of methods or because of facility investment large, or be widely adopted because of production cost Gao Erwei, and traditional steam distillation, little because of its investment, economic benefit is high, still is widely adopted.When steam distillation is produced Bulbus Allii quintessence oil, to pass through the production processes such as screening, immersion, peeling, making beating, enzymolysis, distillation, separation, filtration, these operations all have influence on the output of Bulbus Allii quintessence oil directly or indirectly, and wherein affecting the topmost operation of garlic oil yield is enzymolysis, distillation, three operations of separation.For the enzymolysis operation, CN 200710014402.7, CN 200810195818.8, CN 200310117624.3 etc. have carried out comparatively detailed report; For separation circuit, CN 200310117624.3 and CN 200810016047.1 have reported the method that improves the Bulbus Allii quintessence oil productive rate by improving the measures such as adsorption separation efficiency.But for separation circuit, do not see relevant report.Generally be distillation on producing at present till can not have again obvious essential oil to flow out, but do not take rational technical measures to improve distillation efficiency and then raising garlic oil yield.Therefore, produce at present the upper production technology that distillation efficiency is high, improve the Bulbus Allii quintessence oil yield of being badly in need of improving.
Main citing document:
Yue Tianli etc., to the thinking of China's garlic industrialization development, the Changjiang river vegetables, 2003 (3): 5
200810024407.2 the extracting method of an Oleum Bulbus Allii
200810016047.1 extract the method for garlic essential oil produced with garlic polysaccharide and garlic powder
200310117624.3 unite the method for preparing Bulbus Allii quintessence oil and garlic polysaccharide
200710014402.7 enzyme regulate and control method that improves the Bulbus Allii quintessence oil extraction yield
200810023771.7 the preparation method of a separation and purification Bulbus Allii quintessence oil
200810195818.8 the preparation method of an Oleum Bulbus Allii
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the object of the present invention is to provide a kind of method that improves garlic oil yield, it is accelerated garlicin and changes into the Bulbus Allii quintessence oil composition that is easy to volatilize, and then reduces the distillation energy consumption and improve garlic oil yield.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method that improves garlic oil yield may further comprise the steps:
(1) soak, washing, making beating: be immersed in fresh garlic or dry garlic sheet in the water and stir with impurity such as flush away earth, put again and be broken into granularity on the hollander and starch less than 200 purpose garlics;
(2) enzymolysis: add the allinase active regulator, enzymolysis at room temperature finishes as enzymolysis process when can not check alliin and exist take inspection;
(3) transform: add transforming agent, described transforming agent comprises edible acid, hydrochloric acid, phosphoric acid salt, oxygenant, vitriol, sulfurous acid or sulphite, sodium bicarbonate;
(4) charging, distillation: feed even, solid, avoid forming the steam short circuit, steamer is sealed, and add high flame and distill, Deng having steam to produce and when having distillate to flow out, regulate firepower, control steamer steam generation is 20～30 kg/hours of every side's steamer volumes, and being distilled to does not have till the Bulbus Allii quintessence oil smell in the garlic slag;
(5) essential oil separates: distillate enters rectifying device, and the mixed liquid of the essential oil-water that fractionates out is left standstill in water-and-oil separator, carries out oily water separation, takes out oil phase and is the Bulbus Allii quintessence oil crude product;
(6) Bulbus Allii quintessence oil is refining: the Bulbus Allii quintessence oil crude product by the dry silica gel post, is removed residual water-content and namely got Bulbus Allii quintessence oil.
To soak water weight be 1.5～5 times of fresh garlic weight to fresh garlic in the described step (1), and it is heavy 5～15 times of dry garlic that dry garlic is soaked water weight.
Allinase active regulator composition is blue vitriol, milk of lime, bittern in the described step (2), add-on is that garlic slurry per ton adds blue vitriol 30～50 grams, 1～5 kilogram of 20 degree Beaume milk of lime, 20 degree Beaume bittern, 20～100 grams (main component is the mixture of magnesium chloride, calcium chloride).
Edible acid comprises citric acid, acetic acid, lactic acid in the described step (3); Phosphoric acid salt comprises sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC; Oxygenant comprises potassium permanganate, hydrogen peroxide; Vitriol comprises sodium sulfate, ammonium sulfate, blue vitriol; Sulphite comprises sodium bisulfite, pyrosulfite sodium, sulfurous acid sodium vapor lamp.
The transforming agent addition is 0.05%～3.00% of enzymolysis solution weight in the described step (3).
The theoretical plate number of rectifying device is 5～10 in the described step (5), and gas speed is 0.5～1.5 meter per second and does not add heating unit.
Advantage of the present invention is:
Major advantage of the present invention is after adding suitable transforming agent, can make distillation time shorten 20%, make the output increased of Bulbus Allii quintessence oil to 1-3 doubly, the composition of the Bulbus Allii quintessence oils such as diallyl disulfide, garlicin, diallyl thioether, allyl methyl thioether, allyl methyl disulfide, allyl methyl trisulfide, allyl sulfhydrate, methyl mercaptan is brought up to more than 3 times, sees accompanying drawing 2,3.Another advantage of the present invention is not increase facility investment, can increase in right amount the interpolation transforming agent and get final product on former distillation Bulbus Allii quintessence oil production line.
Know-why of the present invention:
Form in more than the 30 kind of organosulfur compound of Bulbus Allii quintessence oil, difference because of its molecular weight, polarity, solvability equimolecular constitutional features, its volatility is different, such as garlicin, the strongest, the fat-soluble relatively poor and the most difficult volatilization of its polarity (in fact, the garlicin composition has been arranged seldom in the Bulbus Allii quintessence oil product because in gas phase, liquid chromatography separation detection less than).If but can make its rapid conversion become the Bulbus Allii quintessence oil compositions such as diallyl disulfide, garlicin, allyl methyl disulfide, diallyl thioether, allyl methyl thioether, allyl methyl trisulfide, allyl sulfhydrate, methyl mercaptan, then can reduce distillation resistance, the raising distillation efficiency of producing Bulbus Allii quintessence oil; If the selection appropriate measures then can improve in the situation that do not change facility investment the output of Bulbus Allii quintessence oil greatly.
The present invention adopts transforming agents such as adding citric acid, Sodium phosphate dibasic, sodium bicarbonate, accelerate the composition that garlicin changes into the Bulbus Allii quintessence oils such as diallyl disulfide, garlicin, allyl methyl disulfide, diallyl thioether, allyl methyl thioether, allyl methyl trisulfide, allyl sulfhydrate, methyl mercaptan, thereby improve the quality of Bulbus Allii quintessence oil, improve the productive rate of Bulbus Allii quintessence oil.
Known by Fig. 2: when using the transforming agent of 0.05%-0.20%, diallyl organic sulfide content is apparently higher than the processing of not adding transforming agent; Known by Fig. 3: when using the transforming agent of 0.05%-0.20%, allyl methyl organic sulfide content is apparently higher than the processing of not adding transforming agent.Fig. 2,3 measuring methods select ion flow pipe mass spectroscopy (SIFT-MS), and headspace sampling is measured.Determining instrument: Sift voice-100; Condition determination: sweep time: 95 seconds; The Delay computing time: 5 seconds; Each sample determination time: 100 seconds; Sample inlet temperature: 120 ℃; Carrier gas: argon gas; Nebulizer gas pressure: 200KPa; Segregation ratio: 50%; The vacuum flow overpressure; 5Pa.Sampling amount is to be diluted to 80 milliliters after the 2.5 gram garlic making beating, and the sample bottle volume is 1000 milliliters.
Description of drawings
Fig. 1: the schema of producing the Bulbus Allii quintessence oil produced with garlic polysaccharide
Fig. 2: transforming agent is on the impact of generation Bulbus Allii quintessence oil part organosulfur compound, and transforming agent is total amount, contrast: do not add transforming agent, the AM allyl sulfhydrate; The DAS diallyl thioether; The DADS diallyl disulfide; The DATrS garlicin; DATeS diallyl four sulphur.
Fig. 3: transforming agent is on the impact of generation Bulbus Allii quintessence oil part organosulfur compound, and transforming agent is total amount, contrast: do not add transforming agent, the MM methyl mercaptan; AMS allyl methyl thioether; The AMDS allyl methyl disulfide; The MTrS allyl methyl trisulfide; AMTeS allyl methyl four sulphur.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme and the practical situation of the invention described above.
Embodiment 1, carries out in the steps below:
The first step is carried out pre-treatment: fresh garlic clove is placed 5 times of tap water, soaked 2 hours, the impurity such as earth and garlic skin are removed in the flowing water flushing.Control dried open fire, place and be broken into approximately 200 purpose garlics slurry of granularity on the crusher.
Second step makes alliin carry out enzymolysis: (20 degree Beaume bittern 20 restrain for blue vitriol 30 grams, 1 kilogram of 20 degree Beaume milk of lime, and at room temperature enzymolysis is 1 hour, makes alliin be transformed into garlicin fully to add the allinase active regulator by garlic slurry per ton.Finish as enzymolysis process when can not check alliin and exist take inspection.Concrete detection method is: with standard alliin standardized solution, with with enzymolysis garlic juice point on the same silica gel thin sheet, take propyl carbinol: Glacial acetic acid: the mixed liquid of water (4: 1: 1) is as the moving phase chromatography, and take triketohydrindene hydrate as developer, enzymolysis in the garlic juice without till the alliin.
The 3rd step was added transforming agent: add citric acid 0.2%, and SODIUM PHOSPHATE, MONOBASIC 0.1%, ammonium sulfate 0.2% (all calculating with enzymolysis solution weight), transforming agent is used first a small amount of water dissolution, and then enters the charging step after adding enzymolysis solution.
If when carrying out in same container, then adding before distillation, enzymolysis and distillation get final product.
The 4th stepping luggage material, distillation: with the garlic enzymolysis juice steamer of packing into equably, degree of tightness is consistent, avoids forming the steam short circuit; With the steamer sealing, with big fire that steamer is boiled first; Deng having steam to produce and when having distillate to flow out, regulate firepower, control steamer steam generation is 20～30 kg/hours (with every side's steamer volume calculation).Be distilled to and do not have (steamer that loading amount is a ton should distill more than 12 hours) till the Bulbus Allii quintessence oil smell in the garlic slag.
The operation if enzymolysis and distillation when carrying out in same container, then needn't be feeded etc.
The 5th step carried out essential oil and separates: Bulbus Allii quintessence oil and the mixed liquid of water with steamer distills out, at first enter rectifying device, and the theoretical plate number of rectifying device is 5～10, gas speed is 0.5～1.5 meter per second.But do not add heating unit, only utilize the heat energy of steam itself." essential oil-water " that fractionates out mixed liquid is left standstill in water-and-oil separator, carry out oily water separation, take out oil phase and be the Bulbus Allii quintessence oil crude product.
The 6th step made with extra care Bulbus Allii quintessence oil: Oleum Bulbus Allii lentamente by the dry silica gel post, is removed residual water-content and namely got Bulbus Allii quintessence oil, and productive rate is 0.75% (W/W).
Embodiment 2, identical with embodiment 1 first and second, four, five, six steps slightly, from the three step operation different with embodiment 1 be:
Second step adds the allinase active regulator, adds blue vitriol 50 grams by garlic slurry per ton, 3 kilograms of milk of limes, bittern 100 grams.
The 3rd step was added transforming agent: add hydrochloric acid 0.01%, and Sodium phosphate dibasic 2.4%, sodium bisulfite 0.5% (all calculating with the enzymolysis liquid measure), transforming agent is used first a small amount of water dissolution, and then enters the charging step after adding enzymolysis solution.
If enzymolysis and distillation when carrying out in same container, then add before distillation get final product, productive rate is 0.65% (W/W).
Embodiment 3, identical with embodiment 1 first and second, four, five, six steps slightly, from the three step operation different with embodiment 1 be:
Second step adds the allinase active regulator, adds blue vitriol 30 grams by garlic slurry per ton, 2 kilograms of milk of limes, bittern 60 grams.
The 3rd step was added transforming agent: add lactic acid 0.2%, and sodium bicarbonate 0.5%, pyrosulphite hydrogen sodium 0.1% (all calculating with the enzymolysis liquid measure), transforming agent is used first a small amount of water dissolution, and then enters the charging step after adding enzymolysis solution.
Embodiment 4, identical with embodiment 1 first and second, four, five, six steps slightly, from the three step operation different with embodiment 1 be:
The 3rd step was added transforming agent: add sulfurous acid 0.01%, and hydrogen peroxidase 10 .03%, (all calculating with the enzymolysis liquid measure), transforming agent is used first a small amount of water mixing, and then enters the charging step after adding enzymolysis solution.
If when carrying out in same container, then adding before distillation, enzymolysis and distillation get final product, is productive rate 0.73% (W/W)?
Comparative Examples 5, identical with embodiment 1 first and second, four, five, six steps slightly, from the three step operation different with embodiment 1 be:
Second step does not add the allinase active regulator, and the 3rd step was not added transforming agent and garlic ammonia activity regulator.
If when carrying out in same container, then adding before distillation, enzymolysis and distillation get final product.The productive rate of this embodiment only is 0.25% (W/W).
Claims (5)
1. method that improves garlic oil yield is characterized in that may further comprise the steps:
(1) soak, washing, making beating: be immersed in fresh garlic or dry garlic sheet in the water and stir the impurity that comprises earth with flush away, put again and be broken into granularity on the hollander and starch less than 200 purpose garlics;
(2) enzymolysis: add the allinase active regulator, enzymolysis at room temperature finishes as enzymolysis process when can not check alliin and exist take inspection;
(3) transform: add transforming agent, described transforming agent is edible acid, hydrochloric acid, phosphoric acid salt, oxygenant, vitriol, sulfurous acid or sulphite, sodium bicarbonate;
(4) charging, distillation: feed even, solid, avoid forming the steam short circuit, steamer is sealed, and add high flame and distill, Deng having steam to produce and when having distillate to flow out, regulate firepower, control steamer steam generation is 20～30 kg/hours of every side's steamer volumes, and being distilled to does not have till the Bulbus Allii quintessence oil smell in the garlic slag;
(5) essential oil separates: distillate enters rectifying device, and the mixed liquid of the essential oil-water that fractionates out is left standstill in water-and-oil separator, carries out oily water separation, takes out oil phase and is the Bulbus Allii quintessence oil crude product;
(6) Bulbus Allii quintessence oil is refining: the Bulbus Allii quintessence oil crude product by the dry silica gel post, is removed residual water-content and namely got Bulbus Allii quintessence oil;
The transforming agent addition is 0.05%～3.00% of enzymolysis solution weight in the step (3).
2. described a kind of method that improves garlic oil yield according to claim 1 is characterized in that: to soak water weight be 1.5～5 times of fresh garlic weight to fresh garlic in the described step (1), and it is heavy 5～15 times of dry garlic that dry garlic is soaked water weight.
3. described a kind of method that improves garlic oil yield according to claim 1, it is characterized in that: allinase active regulator composition is blue vitriol, milk of lime, bittern in the described step (2), add-on is that garlic slurry per ton adds blue vitriol 30～50 grams, 1～5 kilogram of 20 degree Beaume milk of lime, 20 degree Beaume bittern, 20～100 grams.
4. described a kind of method that improves garlic oil yield according to claim 1, it is characterized in that: edible acid is citric acid, acetic acid, lactic acid in the described step (3); Phosphoric acid salt is sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC; Oxygenant is potassium permanganate, hydrogen peroxide; Vitriol is sodium sulfate, ammonium sulfate, blue vitriol; Sulphite is sodium bisulfite, S-WAT.
5. described a kind of method that improves garlic oil yield according to claim 1, it is characterized in that: the theoretical plate number of rectifying device is 5～10 in the described step (5), and gas speed is 0.5～1.5 meter per second and does not add heating unit.
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| CN102531982A (en) * | 2011-12-23 | 2012-07-04 | 安徽绿能技术研究院 | Method for extracting high purity allicin and device thereof |
| CN103289810B (en) * | 2013-06-09 | 2014-06-18 | 南京工业大学 | Separation and extraction method of garlic oil |
| CN104629905A (en) * | 2013-11-07 | 2015-05-20 | 张湉 | Method used for extracting garlic oil via low-temperature water bath |
| CN103642594A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of garlic oil |
| CN103756932B (en) * | 2013-12-27 | 2015-05-13 | 滕州市悟通香料有限责任公司 | Myroides spp strain and application thereof in preparation of allyl methyl sulfide |
| CN106376911A (en) * | 2016-09-07 | 2017-02-08 | 南阳农业职业学院 | Deodorized fermentation black garlic sauce and preparation method thereof |
| CN109536281A (en) * | 2017-09-22 | 2019-03-29 | 江苏智谋科技有限公司 | A kind of galic essential oil extracting method |
| CN108410581A (en) * | 2018-04-18 | 2018-08-17 | 佛山市飞程信息技术有限公司 | A method of extracting galic essential oil from garlic |
| CN112592765B (en) * | 2020-12-25 | 2022-11-01 | 青岛博恩高科生物技术有限公司 | Preparation method of garlic essential oil |
| CN113122392A (en) * | 2021-04-13 | 2021-07-16 | 吉安市中香天然植物有限公司 | Compound traditional Chinese medicine herbal essential oil and application thereof |
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