CN1261425C - Process for extracting water grind thisvine using alcohole as single organic dissolvent - Google Patents
Process for extracting water grind thisvine using alcohole as single organic dissolvent Download PDFInfo
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- CN1261425C CN1261425C CN 200410025902 CN200410025902A CN1261425C CN 1261425 C CN1261425 C CN 1261425C CN 200410025902 CN200410025902 CN 200410025902 CN 200410025902 A CN200410025902 A CN 200410025902A CN 1261425 C CN1261425 C CN 1261425C
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Abstract
The present invention discloses the process for extracting silymarin by using ethanol as single organic solvent. The process method adopts edible ethanol for extracting silymarin, oil and impurities are removed by the repeated two-time elution with ethanol and water, edible sodium carbonate is used for elution, a silymarin solid obtained by being rinsed in water is dried and then is pulverized, and then a final product is obtained, wherein the content of the total silymarin flavonoid is measured by ultraviolet light, the mass percentage concentration is from 70 to 90 %, and the yield of a product is 2 to 3 % of a silymarin seed of which the oil is squeezed. The present invention solves the problem of harmful solvent residue in the present silymarin product, and a silymarin product without harmful solvent residue can be obtained by the extracted process.
Description
Technical field
The present invention relates to traditional Chinese medical science pharmacy field, relate in particular to from natural product herbal medicine separation and Extraction monomer medicine with the silymarin extraction process of ethanol as single organic solvent.
Background technology
Silymarin is the general name of the Flavonoid substances that extraction separation goes out from the seed of natural product Silymarin, has mainly comprised 5 kinds of Flavonoid substances such as silibinin, Isosilybin.That silymarin has is anti-oxidant significantly, remove effect such as free radical, is mainly used at present in the treatment of hepatopathy, and secondly, silymarin also has significant curative effect for the some diseases of cardiovascular systems such as hyperlipidemia etc.
The early stage ethyl acetate that adopts that is extracted in of silymarin is carried out more, silymarin adopts acetone to extract from the Silymarin seed mostly at present, carry out degreasing with sherwood oil or hexane etc. then, obtain yellow or yellowish powder-product, the comparative study report that adopts methyl alcohol to extract is also arranged.Do not see at present that both at home and abroad correlative study or patent report are arranged and there is the residual Silymarin extraction process of hazardous solvent.
In recent years, because the human consumer of the U.S., Europe, Japan is more and more stricter for the requirement of solvent residual amount, not only there is dissolvent residual in the plant milk extract that adopts present methyl alcohol, acetone, sherwood oil, ethyl acetate, hexane etc. can cause the organic solvent separation and Extraction of certain murder by poisoning to obtain to human body, but also the problem that often exists residual solvent to exceed standard.
Summary of the invention
The objective of the invention is to overcome the shortcoming of the above hazardous solvent residue that in the silymarin leaching process, exists, propose a kind of with the silymarin extraction process of ethanol as single organic solvent.Extraction process of the present invention only adopts ethanol as single organic solvent, adopts gradient method technology, has solved the dissolvent residual problem in the silymarin.
Technical scheme of the present invention adopts extraction using alcohol to fly the processing method of silibin, may further comprise the steps:
1) with the oil expression of Silymarin seed process, oil yield is about 15% of the preceding seed weight of oil expression, presses into the oil cake that thickness is 1-3mm;
2) the Silymarin oil cake powder that will press oil is broken into the extractor of packing into after 20 orders sieve, and the edible ethanol that adds concentration and be 85%-95% is heated to the boiling back and keeps constant temperature backflow 1.5-3 hour to flooding height of materials, extracts 3-5 time continuously;
3) concentration tank of will the Silymarin extracting solution behind extraction using alcohol packing into concentrates, when ethanol content in the concentrated solution through the alcoholic degree instrumentation fixed less than 10% after, emit concentrated solution, concentrated solution is cooled to below 40 degrees centigrade, emit the upper liquid vegetables oil, the solids of bottom with the hot water injection more than 60 degrees centigrade, is removed the part grease of solid surface;
4) in the gained solids, add the softening water of 5 times of weight, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, emit supernatant liquid then, stay solids;
5) ethanol of 3-5 times of weight concentration 10%-50% of adding in above gained solids keeping 30 minutes to 2 hours more than 70 degrees centigrade, is emitted supernatant liquid then, stays solids;
6) in above gained solids, add the softening water of 2-5 times of weight, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, pour out supernatant liquid then, stay solids;
7) ethanol of 3-5 times of weight concentration 10%-50% of adding in above gained solids kept 30 minutes to 2 hours at constant temperature more than 70 degrees centigrade, poured out supernatant liquid then, stayed solids;
8) in above gained solids, add 2-5 times of weight softening water, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, pour out supernatant liquid then, stay solids;
9) in above gained solids, add mass percent concentration be 0.1%-2% edible sodium carbonate solution 1-5 doubly, keeping 10 minutes to 2 hours more than 60 degrees centigrade, pour out supernatant liquid then, again with 3-10 doubly measure, hot water more than 70 degrees centigrade carries out rinsing and removes edible yellow soda ash, after the solids drying of gained, pulverize and promptly obtain no solvent residue silymarin the finished product.
The silibin process for extracting that flies of the present invention can obtain not having the residual silymarin product of hazardous solvent, Herba Silybi mariani total flavones content is mass percent 70%-90% through the result of ultraviolet determination in the product, product yield was for pressing the 2%-3% of oil back Silymarin seed, and ethanol content is less than 0.5% in the product.
Description of drawings
Fig. 1 is the technical process diagram of the residual silymarin extraction process of no hazardous solvent.
Embodiment
Below in conjunction with accompanying drawing technical process of the present invention is done further to describe in detail.
At first adopt the ethanol of 8-15 times of weight from press oil back Silymarin seed, to carry out the silymarin extraction, after again extract being concentrated, be cooled to room temperature range, separate then and remove the Silymarin oil on top, the solid matter that the bottom is settled out adds softening water or the deionized water that 1-5 doubly measures, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, pour out supernatant liquid then, the ethanol that in the solids of bottom, adds the 10%-50% mass percent, after heating keeps refluxing 30 minutes to 2 hours, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, and then with aforesaid Ethanol Treatment method, handle the back adds 0.1%-2% (mass percent concentration) in the gained solids edible sodium carbonate solution 1-5 times, kept 10 minutes to 2 hours more than 60 degrees centigrade, pour out supernatant liquid then, doubly measuring more than 70 degrees centigrade hot water with 3-10 again carries out rinsing and removes edible yellow soda ash, pulverize behind the solid drying of gained and promptly obtain the finished product, wherein Herba Silybi mariani total flavones content is through ultraviolet determination, mass percent concentration is 70%-90%, and product yield was for pressing oil back Silymarin seed 2%-3%.In carrying out silymarin extraction process process, the order the when yellow soda ash that is added and ethanol oil removing and impurity can carry out the conversion of order successively.
Embodiment 1: at first the Silymarin seed is pressed into the oil cake that thickness is 1.5mm, being ground into the 20 orders back of sieving measures 85% ethanol with 4 times in oil cake and carries out refluxing extraction, extract altogether four times, after again extracting solution being concentrated, be cooled to 30 degrees centigrade, separate then and remove the Silymarin oil on top, the solid matter that the bottom is settled out adds the deionized water of 3 times of amounts, heated and stirred to 80 degree centigrade, kept 30 minutes, pour out supernatant liquid then, in the solids of bottom, add the ethanol of 3 times of amounts 15%, after heating keeps refluxing 1 hour, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, and then with aforesaid Ethanol Treatment method, handles the back adds 0.1%-2% (mass percent concentration) in the gained solids 3 times of edible sodium carbonate solutions, 70 degrees centigrade kept 20 minutes, pour out supernatant liquid then, the hot water with 80 degrees centigrade of 5 times of amounts carries out rinsing again, pulverizes behind the solid drying of gained and promptly obtains the finished product.
Embodiment 2: at first the Silymarin seed is pressed into the oil cake that thickness is 2mm, pulverizing the 20 orders back of sieving measures 90% ethanol with 3 times and carries out refluxing extraction, extract altogether three times, after again extracting solution being concentrated, be cooled to 35 degrees centigrade, separate then and remove the Silymarin oil on top, the solid matter that the bottom is settled out adds the deionized water of 5 times of amounts, heated and stirred to 85 degree centigrade, kept 30 minutes, and poured out supernatant liquid then, in the solids of bottom, add the ethanol of 3 times of amounts 25%, after heating keeps refluxing 40 minutes, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, adds 4 times of the edible sodium carbonate solutions of 0.1%-2% (mass percent concentration) in the gained solids, 75 degrees centigrade kept 40 minutes, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, and then with aforesaid Ethanol Treatment method, carry out rinsing with 4 times of hot water of measuring 85 degrees centigrade again after handling, pulverize behind the solid drying of gained and promptly obtain the finished product.
Embodiment 3: at first the Silymarin seed is pressed into the oil cake that thickness is 2.5mm, pulverizing the 20 orders back of sieving measures 95% ethanol with 4 times and carries out refluxing extraction, extract altogether four times, after again extracting solution being concentrated, be cooled to 30 degrees centigrade, separate then and remove the Silymarin oil on top, the solid matter that the bottom is settled out adds the deionized water of 4 times of amounts, heated and stirred to 90 degree centigrade, kept 20 minutes, and poured out supernatant liquid then, in the solids of bottom, add the ethanol of 2.5 times of amounts 25%, after heating keeps refluxing 30 minutes, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, adds 3 times of the edible sodium carbonate solutions of 0.1%-2% (mass percent concentration) in the gained solids, 80 degrees centigrade kept 30 minutes, pour out supernatant liquid then, bottom solids water is again done aforementioned processing, and then with aforesaid Ethanol Treatment method, carry out rinsing with 3 times of hot water of measuring 90 degrees centigrade again after handling, pulverize behind the solid drying of gained and promptly obtain the finished product.
The invention solves the hazardous solvent residue problem in the present silymarin product, can obtain not having the residual silymarin product of hazardous solvent by extraction process of the present invention, Herba Silybi mariani total flavones content is mass percent 70%-90% through the result of ultraviolet determination in the product, product yield was for pressing the 2%-3% of oil back Silymarin seed, and ethanol content is less than 0.5% in the product.
Claims (4)
1, a kind of with the silymarin extraction process of ethanol as single organic solvent, it is characterized in that this process using ethanol as single organic solvent separation and Extraction silymarin, may further comprise the steps:
1) with the oil expression of Silymarin seed process, oil yield is about 15% of the preceding seed weight of oil expression, presses into oil cake;
2) the Silymarin oil cake powder that will press oil is broken into the extractor of packing into after 20 orders sieve, and the ethanol that adds concentration and be 85%-95% is heated to the boiling back and keeps constant temperature backflow 1.5-3 hour to flooding height of materials, extracts 3-5 time continuously;
3) concentration tank of will the Silymarin extracting solution behind extraction using alcohol packing into concentrates, when ethanol content in the concentrated solution through the alcoholic degree instrumentation fixed less than 10% after, emit concentrated solution, concentrated solution is cooled to below 40 degrees centigrade, emit the upper liquid vegetables oil, the solids of bottom with the hot water injection more than 60 degrees centigrade, is removed the part grease of solid surface;
4) in the gained solids, add the softening water of 5 times of weight, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, emit supernatant liquid then, stay solids;
5) ethanol of 3-5 times of weight concentration 10%-50% of adding in above gained solids keeping 30 minutes to 2 hours more than 70 degrees centigrade, is emitted supernatant liquid then, stays solids;
6) in above gained solids, add the softening water of 2-5 times of weight, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, pour out supernatant liquid then, stay solids;
7) ethanol of 3-5 times of weight concentration 10%-50% of adding in above gained solids kept 30 minutes to 2 hours at constant temperature more than 70 degrees centigrade, poured out supernatant liquid then, stayed solids;
8) in above gained solids, add 2-5 times of weight softening water, more than the heated and stirred to 70 degree centigrade, kept 30 minutes to 2 hours, pour out supernatant liquid then, stay solids;
9) adding 1-5 mass percent concentration doubly in above gained solids is the edible sodium carbonate solution of 0.1%-2%, keeping 10 minutes to 2 hours more than 60 degrees centigrade, pour out supernatant liquid then, again with 1-10 doubly measure, hot water more than 70 degrees centigrade carries out rinsing and removes edible yellow soda ash, after the gained solids drying, pulverize and promptly obtain no solvent residue silymarin the finished product.
2, according to claim 1 with the silymarin extraction process of ethanol as single organic solvent, it is characterized in that said ethanol is edible ethanol.
3, according to claim 1 with the silymarin extraction process of ethanol as single organic solvent, it is characterized in that said oil cake thickness is 1-3mm.
4, according to claim 1 with the silymarin extraction process of ethanol as single organic solvent, the order when it is characterized in that adding yellow soda ash and ethanol oil removing and impurity can successively be changed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410025902 CN1261425C (en) | 2004-03-03 | 2004-03-03 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410025902 CN1261425C (en) | 2004-03-03 | 2004-03-03 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
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| Publication Number | Publication Date |
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| CN1560046A CN1560046A (en) | 2005-01-05 |
| CN1261425C true CN1261425C (en) | 2006-06-28 |
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| CN 200410025902 Expired - Fee Related CN1261425C (en) | 2004-03-03 | 2004-03-03 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381363B (en) * | 2007-09-06 | 2010-11-03 | 天津大学 | Method for extracting macroporous adsorption resin and separating hepadestal from alkaline water |
| CN102079745B (en) * | 2009-12-01 | 2013-09-11 | 白心亮 | Production method of silymarin |
| CN102293804B (en) * | 2010-06-25 | 2013-06-05 | 北京京卫燕康药物研究所有限公司 | Optimized scheme for comprehensively utilizing silybum mariamum |
| CN102558162A (en) * | 2010-12-20 | 2012-07-11 | 佳木斯三江水飞蓟素制品有限公司 | Processing and extraction method for silybin with low soluble residues and high content |
| CN102964342B (en) * | 2012-12-18 | 2015-05-13 | 佳木斯三江水飞蓟素制品有限公司 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
| CN102993187A (en) * | 2012-12-24 | 2013-03-27 | 王振奎 | Method for extracting silymarin by nitrogen protection |
| CN103408538B (en) * | 2013-08-27 | 2015-06-24 | 白心亮 | Method for extracting silymarin |
| CN103408539B (en) * | 2013-08-28 | 2016-04-06 | 天津泰阳制药有限公司 | The production method of high-purity silymarin |
| CN104650050B (en) * | 2014-01-17 | 2019-03-15 | 吴长军 | It is a kind of with the silymarin extracting method that food grade ethyl alcohol is Extraction solvent |
| CN105859699A (en) * | 2016-04-08 | 2016-08-17 | 江苏健佳药业有限公司 | Preparation method of silymarin |
| CN108456199A (en) * | 2017-02-20 | 2018-08-28 | 南京宸翔医药研究有限责任公司 | A kind of production technology, pharmaceutical composition and its clinical application of high-purity silymarin meglumine |
| CN108578263A (en) * | 2018-06-20 | 2018-09-28 | 吉林农业科技学院 | Silymarin Skin whitening care cosmetics |
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