CN1234828C - Process for extracting coix seed oil by using supercritical CO2 extraction method - Google Patents
Process for extracting coix seed oil by using supercritical CO2 extraction method Download PDFInfo
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- CN1234828C CN1234828C CN 02145332 CN02145332A CN1234828C CN 1234828 C CN1234828 C CN 1234828C CN 02145332 CN02145332 CN 02145332 CN 02145332 A CN02145332 A CN 02145332A CN 1234828 C CN1234828 C CN 1234828C
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- coix seed
- seed oil
- semen coicis
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Abstract
The present invention discloses a method of extracting coix seed oil by supercritical carbon dioxide. The present invention matches carbon dioxide under a supercritical state with entrainer to extract coix seed, and the yield rate reaches over 8.18%, which is higher than the coix seed oil yield disclosed in the prior art. The extracted coix seed oil is analyzed by a GC-MC method, and the fatty acid content of the obtained coix seed oil ingredients and the fatty acid content disclosed in the prior art are approximately same. The method of the present invention can keep active ingredients of the coix seed oil free from loss, and is convenient for industrialized extraction of the coix seed oil. Because the coix seed oil contains large numbers of other ingredients of unsaturated fatty acids, proteins, etc., the coix seed oil can be made into medicines for treating cancer, regulating immunity, reducing blood lipid, resisting inflammation, relieving cough, etc., simultaneously can be used for developing functional foods of anti-aging, fatigue resistance, beauty treatment, health care, etc., and has wide application prospects and very high economic values.
Description
Technical field
The present invention relates to a kind of method of Semen Coicis oil, particularly a kind of method that adopts the supercritical carbon dioxide extraction Semen Coicis oil.
Background technology
Semen Coicis is the dry mature kernal of grass Coix lacrymajoib L.var.mayuen (Roman) Stapf, and sweet, light, the cool invigorating the spleen excreting dampness of distinguishing the flavor of removes numbness and quenches the thirst clearing away heat and eliminating pus.Wherein contain a large amount of unsaturated fatty acidss in the Semen Coicis oil, be used for treatment for cancer clinically.The method of traditional extraction Semen Coicis oil is the organic solvent soaking extraction method, and used solvent is generally sherwood oil or ether etc.Described method is operated numerous defectives, need a large amount of organic solvents, be generally 100～150 times that extract material, contain more impurity in the extract, brought certain difficulty not only for the separated and collected of postorder, and certain organic solvent residual is often arranged in extract, limited and extracted the application of goods in industries such as medicine, food.Supercritical carbon dioxide extraction method is a kind of brand-new, the efficient separating substances technology that chemical field researchdevelopment in nearly 20 years is got up, this technology biggest advantage is that carbonic acid gas is as spe medium, nontoxic, can there be dissolvent residual and environmental pollution, because extraction is to carry out, can prevent oxidation, the Denaturation of the oil that extracts under anaerobic state.
" Chinese medicinal materials " 22 the 8th phases of volume disclose a kind of method of supercritical carbon dioxide extraction Semen Coicis oil, but its yield is 4.31% only, is difficult to apply.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of method of supercritical carbon dioxide extraction Semen Coicis oil, overcome the lower defective of Semen Coicis oil yield that prior art exists.
Technical conceive of the present invention is such:
The carbonic acid gas that the present invention will be under the supercritical state cooperates with entrainment reagent, and Semen Coicis is extracted, and makes the oil in the Semen Coicis be able to abundant dissolving, thereby can obtain higher yield.
Method of the present invention comprises the steps:
With CO
2Gas and entrainment reagent feed in the extractor that is equipped with Semen Coicis continuously;
Extracted the CO of Semen Coicis oil
2Gas and entrainment reagent enter the extraction-container step-down and resolve;
Adopt conventional method from the parsing thing that contains entrainment reagent and Semen Coicis oil, to collect Semen Coicis oil, CO
2Gas recycles after pressurization.
The present invention also can carry out according to following steps:
With CO
2Gas feeds in the extractor that is equipped with entrainment reagent and Semen Coicis continuously;
Extracted the CO of Semen Coicis oil
2Gas and entrainment reagent are sent into the extraction-container step-down and are resolved;
Adopt conventional method from the parsing thing that contains entrainment reagent and Semen Coicis oil, to collect Semen Coicis oil, CO
2Gas recycles after pressurization.
The entrainment reagent of being addressed can adopt water, ethanol or aqueous ethanolic solution.
The present invention passes through to add entrainment agent, and selects the kind and the consumption of suitable entrainment agent, and determines best temperature and pressure condition, and this extraction yield is reached more than 8.18%, is higher than the yield of the disclosed Semen Coicis oil of prior art.The Semen Coicis oil that extracts is carried out GC-MC to be analyzed, disclosed roughly the same in the content of lipid acid and the prior art in the composition of resulting Semen Coicis oil, proof present method can keep in the Semen Coicis oil activeconstituents not suffer a loss, and is a kind of method that Semen Coicis oil is extracted in industrialization of being convenient to.
Description of drawings
Fig. 1 is the schema of supercritical carbon dioxide extraction Semen Coicis oil of the present invention.
Embodiment
Referring to Fig. 1, method of the present invention comprises the steps:
With CO
2Gas and entrainment reagent feed in the extractor 1 that is equipped with Semen Coicis continuously;
Extracted the CO of Semen Coicis oil
2Gas and entrainment reagent send into first extraction-container 2 and 3 step-downs of second extraction-container are resolved;
Adopt conventional method from the parsing thing that contains entrainment reagent and Semen Coicis oil, to collect Semen Coicis oil, CO
2Recycle after compressed machine 4 pressurizations of gas.
The per hour flow of entrainment reagent is the 30%-60% of Semen Coicis weight.
According to the present invention, also can be with CO
2Gas feeds in the extractor 1 that is equipped with entrainment reagent and Semen Coicis continuously, will extract the CO of Semen Coicis oil then
2Gas and entrainment reagent are sent into the extraction-container step-down and are resolved;
The entrainment reagent of being addressed can adopt water, ethanol or aqueous ethanolic solution, and the concentration of aqueous ethanolic solution is 30～90wt%.
According to the present invention, preferably earlier with its pulverizing, granularity is controlled below 60 orders;
Extraction temperature is 40-60 ℃, and pressure is 15-30MPa; The temperature of first extraction-container 2 is 40-55 ℃, and pressure is 6-12MPa; The temperature of second extraction-container 3 is 45-50 ℃, and pressure is 4-7Mpa, CO
2Flow be the 100-400Kg/h.Kg Semen Coicis, the extraction time is 3-4 hour, the entrainment reagent consumption is the 30%-60% of Semen Coicis weight.
Embodiment 1
Be crushed to 60 purpose Semen Coiciss and 0.6 kilogram of aqueous ethanolic solution input extractor 1 that concentration is 70wt% with 2 kilograms, the control extraction temperature is 42 ℃, and extracting pressure is 20Mpa, and first extraction-container, 2 temperature are 45 ℃, pressure is 10Mpa, the temperature of second extraction-container 3 is 40 ℃, and pressure is 6Mpa, and the flow of carbonic acid gas is 200kg/h, extract after 4 hours, from first extraction-container 2 and second extraction-container 3, take out to resolve extract, i.e. Semen Coicis oil, yield is 8.18%.
Embodiment 2
Be crushed to 50 purpose Semen Coiciss with 5 kilograms and drop into extractor, the control extraction temperature is 40 ℃, and pressure is 8MPa, and first resolution temperature is 44 ℃, and second resolution temperature is 41 ℃, feeds CO
2Gas, and pump into entrainment agent ethanol, the alcoholic acid flow is 1500 gram/h, and the first parsing pressure is 9MPa, and the second parsing pressure is 5MPa, extracts after 3.3 hours, takes out extract from first extraction-container and second extraction-container, is Semen Coicis oil, and yield is 7.22%.
Embodiment 3
The GC-MS of fatty acid content analyzes in the Semen Coicis oil
1, the preparation of test sample:
To place container through 0.1 gram of the Semen Coicis oil behind the carbon dioxide abstraction, add 1ml methyl alcohol and 1ml0.8mol/LKOH-methyl alcohol, shake gently 5 minutes, add entry, and get supernatant liquor and carry out the GC-MS analysis to 10ml.
2, test conditions:
The GC condition is as follows: chromatographic column FFAP25mm * 0.2mm quartz capillary column, 150 ℃ of column temperatures, are pressed 50kPa by 10 ℃/min before 250 ℃ of the injector temperatures, post.
The MS condition is as follows: EI ion source, ion energy 70eV, electron-multiplier high pressure 1900V, 200 ℃ of amu of mass scanning.
3, test method:
Operation according to a conventional method.
4, test-results:
Mass spectrum identifies four kinds of lipid acid by retrieval, measures their relative content with area normalization method, and is as follows: palmitinic acid, 18.5%; Linolic acid, 30.8%; Oleic acid, 45.6%; Stearic acid, 2.1%.
Claims (3)
1. the method for a supercritical carbon dioxide extraction Semen Coicis oil is characterized in that comprising the steps:
With CO
2Gas and entrainment reagent feed in the extractor (1) that is equipped with Semen Coicis continuously;
Extracted the CO of Semen Coicis oil
2Gas and entrainment reagent send into first extraction-container (2) and second extraction-container (3) step-down is resolved;
Adopt conventional method from the parsing thing that contains entrainment reagent and Semen Coicis oil, to collect Semen Coicis oil;
Extraction temperature is 40-60 ℃, and pressure is 15-30MPa; The temperature of first extraction-container (2) is 40-55 ℃, and pressure is 6-12MPa; The temperature of second extraction-container (3) is 45-50 ℃, and pressure is 4-7Mpa, and the flow of CO2 is the 100-400Kg/h.Kg Semen Coicis, and the extraction time is 3-4 hour, and the entrainment reagent consumption is the 30%-60% of Semen Coicis weight;
The entrainment reagent of being addressed is a water;
The per hour flow of entrainment reagent is the 30%-60% of Semen Coicis weight.
2. method according to claim 1 is characterized in that recycling after the compressed machine of CO2 gas (4) pressurization.
3. method according to claim 1 is characterized in that earlier coix seed powder being broken to below 60 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02145332 CN1234828C (en) | 2002-11-21 | 2002-11-21 | Process for extracting coix seed oil by using supercritical CO2 extraction method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02145332 CN1234828C (en) | 2002-11-21 | 2002-11-21 | Process for extracting coix seed oil by using supercritical CO2 extraction method |
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| Publication Number | Publication Date |
|---|---|
| CN1502680A CN1502680A (en) | 2004-06-09 |
| CN1234828C true CN1234828C (en) | 2006-01-04 |
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| CN 02145332 Expired - Fee Related CN1234828C (en) | 2002-11-21 | 2002-11-21 | Process for extracting coix seed oil by using supercritical CO2 extraction method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103689126A (en) * | 2013-12-05 | 2014-04-02 | 明光市鸿远油脂有限公司 | Edible healthcare rapeseed oil for dispelling wind and removing obstruction in the meridians |
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| EP1792542A1 (en) * | 2005-12-02 | 2007-06-06 | SCF Technologies A/S | A method for producing a prepared food product having a reduced content of species |
| CN101036761B (en) * | 2007-04-23 | 2010-05-19 | 肖志勇 | Process for preparing coix seed oil |
| CN102229855B (en) * | 2011-06-05 | 2013-06-19 | 江苏江大源生态生物科技有限公司 | Method for extracting coix seed oil by supercritical CO2 extraction and rectification |
| DK2937095T3 (en) * | 2012-12-20 | 2017-09-11 | Joben Bio-Medical Co Ltd | EXTRACT OF COIX LACRYMA JOBI SEEDLY AND USE THEREOF |
| TWI541017B (en) | 2012-12-20 | 2016-07-11 | 喬本生醫股份有限公司 | Extract of adlay bran and uses thereof |
| CN104146079A (en) * | 2014-07-14 | 2014-11-19 | 和县绿源油脂有限公司 | Whitening and anti-wrinkle rapeseed oil |
| CN105311486A (en) * | 2014-07-18 | 2016-02-10 | 浙江康莱特集团有限公司 | Coix seed oil containing 16 glycerides, preparation and applications thereof |
| CN105250804A (en) * | 2014-07-18 | 2016-01-20 | 浙江康莱特集团有限公司 | Coix seed oil containing 11 triglycerides, preparation and applications thereof |
| US9585929B2 (en) * | 2014-07-18 | 2017-03-07 | Zhejiang Kanglaite Group Co., Ltd. | Coix seed oil containing 13 glycerides, and pharmaceutical preparation and use thereof |
| US9585858B2 (en) * | 2014-07-18 | 2017-03-07 | Zhejiang Kanglaite Group Co., Ltd. | Pharmaceutical composition containing 13 triglycerides, and preparations and use thereof |
| CN105018219A (en) * | 2015-06-29 | 2015-11-04 | 广西大学 | Method for supercritical CO2 extraction of coix seed oil |
| CN106421540A (en) * | 2016-12-28 | 2017-02-22 | 四川默森药业有限公司 | Patch for soft tissue damage and preparation method of patch |
| WO2021050000A1 (en) * | 2019-09-12 | 2021-03-18 | Crop Protection (Singapore) Pte. Ltd. | Method of preparing patchouli extract |
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2002
- 2002-11-21 CN CN 02145332 patent/CN1234828C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103689126A (en) * | 2013-12-05 | 2014-04-02 | 明光市鸿远油脂有限公司 | Edible healthcare rapeseed oil for dispelling wind and removing obstruction in the meridians |
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| Publication number | Publication date |
|---|---|
| CN1502680A (en) | 2004-06-09 |
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