CN1504486A - Extracting technology for mountain ophiopogon root polysaccharide - Google Patents
Extracting technology for mountain ophiopogon root polysaccharide Download PDFInfo
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- CN1504486A CN1504486A CNA021477582A CN02147758A CN1504486A CN 1504486 A CN1504486 A CN 1504486A CN A021477582 A CNA021477582 A CN A021477582A CN 02147758 A CN02147758 A CN 02147758A CN 1504486 A CN1504486 A CN 1504486A
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Abstract
The invention discloses a process for extracting liriope spicata lour polysaccharides comprising the steps of, A. using liquid phase chromatogram-mass spectrometer to select liriope spicata lour medicinal material whose root tuber has the similar component and content as the standard medicinal materials, B. producing the selected root tuber into coarse powder, coarse powder displacement using ethanol, C. removing alcohol from slag, extracting through water-bath, D. combining and concentrating the filter liquor, alcohol separating, E. vacuum drying of alcohol separated deposition, chalking in to obtain powder form liriope spicate lour polysaccharide extract, F. measuring the content of liriope spicate lour polysaccharide in the extract through spectrophotometry.
Description
Technical field
The invention belongs to a kind of method of extracting vegetable polysaccharides, especially a kind of method of from the Chinese medicinal materials Radix Liriopes, extracting polysaccharide.
Background technology
The conventional method of extracting vegetable polysaccharides be earlier with 95% ethanol (or methyl alcohol) heating and refluxing extraction removing interference compositions such as monose, oligose, glucoside, and then add repeatedly extracting polyose composition wherein of water.
Several scholar's research of Zhejiang College Of Traditional Chinese Medicine affiliated hospital (see publish Zhejiang College Of Traditional Chinese Medicine journal in February, 1999 the 23rd the 1st phase of volume the 59th page to 60 pages) are thought: because Radix Ophiopogonis polysaccharide mainly is made up of glucose and fructose, composition is fairly simple, extracting method with routine adds the alcohol reflux removal of impurities earlier, again with the as easy as rolling off a log polyose composition depolymerization that causes wherein of water extraction, precipitation is separated out less even is not had during alcohol precipitation.They have proposed an improved processing method: earlier with ethanol diacolation in the diacolation device of 90%, carry 3 times with well-established law water then, filtrate is concentrated into 1/10 after adding active carbon purifying, add 95% alcohol chromatography again, the precipitation separated out with behind the dehydrated alcohol, acetone, ether washing 5 times in 60 ℃ of oven dry, the yield 1% of gained Radix Ophiopogonis polysaccharide amorphous powder.From the data of its announcement, the content of Radix Ophiopogonis polysaccharide is 59%-61% in the extract.
The diacolation method that this institute proposes obviously is better than conventional reflux method, but they do not find best processing condition, wherein some processing condition is provided with unreasonable, therefore the yield of the Radix Ophiopogonis polysaccharide of gained too low (only 1%), in its extract the content of polysaccharide not high yet (only be 59%-61%, adopt ordinary method can reach 50%-70%), and alcohol analyses the back and uses the organic solvent washing throw out, is unfavorable to the Radix Ophiopogonis polysaccharide as drug use.
In addition, choosing of Chinese medicinal materials is an open question still always, has a kind of suggestion to think that the medicinal material that this active constituent content is high is excellent medicinal material with one or two effective constituent in the chemico-analytic method mensuration Chinese medicinal materials.Another kind of suggestion thinks that the quality of Chinese medicinal materials answers the analysis-by-synthesis evaluation, is example with the genseng, and the content of ginsenoside is very high in the genseng of cultivation, even also higher than wild ginseng's content, but the pharmaceutical use of the genseng of artificial growth can not show a candle to the wild ginseng; In the Chinese medicinal materials except known effective constituent, the existence of other submember whether and what of content be prior factor sometimes.Therefore, the technology of extracting chemical substance from Chinese medicinal materials of a reasonable optimizing should at first be started with from choosing medicinal material, and not only do not choose medicinal material in the technology of above-mentioned Zhejiang institute of traditional Chinese medicine, and it adopts when carrying out diacolation is the piece root of the tuber of dwarf lilyturf, and this is disadvantageous to the effective constituent in this medicinal material of abundant extraction.
At Chinese materia medica circle, traditional method of choosing medicinal material is to choose medicinal material according to plant taxonomy, and of requirement and people's experience decides the grade of medicinal material.This method randomness, empirical too strong, non-quantitative, operability is too poor.Under no professional pharmacy personnel's situation, how other personnel correctly choose medicinal material also is a new problem that is worth exploration.
Summary of the invention
Above-mentioned deficiency at prior art, the objective of the invention is to propose a kind of simple, reasonable quantifiable processing method, the extract that uses present method to extract from Radix Liriopes can account for 30% of medicinal material dry weight, and the purity of extract is also very high, its sugar contents can reach 90%, and wherein the content of polysaccharide is generally 73%-87%.
The object of the present invention is achieved like this: the extraction process of Radix Liriopes polysaccharide is carried out according to following steps in order:
A, be benchmark, use high performance liquid chromatography-GC-MS, choose piece root with standard medicinal ingredient, Radix Liriopes that content is close according to medicinal materials fingerprint with the control medicinal material of national Nat'l Pharmaceutical ﹠ Biological Products Control Institute;
B, with the Radix Liriopes piece root chosen clean, dry, the levigate Radix Liriopes meal that is prepared as, with ethanol diacolation in the diacolation device of Radix Liriopes meal and 5-7 times 90%;
C, the dregs of a decoction go to the alcohol back to extract 2 times each 20-40 minute with 8-12 times of water in 70-98 ℃ of water-bath;
D, filtrate are concentrated into 1/10 of original volume after merging, and add 95% ethanol, and making pure content is 80% o'clock, and alcohol is analysed;
E, beat powder after 50 ℃ of vacuum-drying, resulting powder is the Radix Liriopes polyoses extract that is extracted.
The content of Radix Liriopes polysaccharide in F, the usefulness spectrophotometry extract.
The Radix Liriopes meal of extraction process is with in the ethanol percolation operation, and consumption of ethanol doubly is good with 5.5-6.5, and the best is 6 times.
The dregs of a decoction in the extraction process go in the extracting in water operation of alcohol back, and the consumption of water doubly is good with 9-11, and optimum amount is 10 times; Extracting temperature is good with 75-90 ℃, and optimum temps is 85 ± 2 ℃; The optimum extraction number of times is 2 times; Each extraction time is 30min.
Described vacuum drying optimum temps is 50 ± 2 ℃.
The instruments such as can also adopting liquid chromatography, infrared spectra of choosing to the raw material Radix Liriopes in the extraction process carries out.
Craft science proposed by the invention, rationally, have innovative idea and achieve noticeable achievement.As everyone knows, the quality good or not of differentiating Chinese medicinal materials is a special technical ability, past mainly is to be undertaken by the personnel that special experience is arranged, this " artificial identification " often is difficult for being admitted by modern science, the present invention proposes a instrument and carry out the technical measures that Chinese medicinal materials is differentiated (choosing) with modern science, its standard medicinal material is that the professional chooses with the artificial comprehensive judgement, other medicinal material comes and the comparison of standard medicinal material with the method for Instrument measuring, such method both communicated with modern science, the truth that can reflect Chinese medicinal materials again is a rare revolutionary approach.
The present invention has chosen the processing condition of series of optimum, the yield and the content of Radix Liriopes polysaccharide are significantly improved, and the extract that present method is extracted from Radix Liriopes can account for 30% of medicinal material dry weight, and the content of polysaccharide is very high, the content of polysaccharide is generally 73%-87%, and sugar contents can reach 90%.High like this extraction yield and content have proved the reasonableness and the advance of technology of the present invention.The present invention does not adopt organic solvent that pure hypostasis is washed, and has reduced artificial pollution.
The vacuum drying processing method that the present invention adopts is to the general better drying means of insoluble compound in the prior art, the drying that this method is used for the Radix Liriopes polyoses extract is a reasonably transplanting, it is good with Radix Liriopes polyoses extract drying that it can guarantee under lower temperature, because the low side reaction that other can not take place of drying temperature, the performance of dry thing is also better.
Description of drawings
Accompanying drawing 1 is the process flow sheet of the embodiment of the invention;
Accompanying drawing 2 is high performance liquid chromatography-mass spectroscopy collection of illustrative plates of standard Radix Liriopes medicinal material;
Accompanying drawing 4 is diacolation device diacolation synoptic diagram.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is described in further detail.Below be described according to the order of technological process and step:
A, at first chooses the Radix Liriopes medicinal material with high performance liquid chromatography-GC-MS, and the used medicinal material of the present invention is that Radix Liriopes is produced in Hubei.Adopt high performance liquid chromatography-mass spectroscopy, obtain total ions chromatogram, the retention time at each peak and peak area in the scaling system, methodological study by stability, circulation ratio, precision, choose relative standard deviation (RSD value) less than 17 peaks of 5% as characteristic peak, set up the characteristic fingerprint pattern of Radix Liriopes medicinal material thus.Same method is measured the retention time and the area of 17 peak values of the material of getting it filled to be selected.Adopt computer multivariate statistics software to carry out cluster analysis, calculate the similarity (distance) of get it filled material and standard medicinal material to be selected and make dendrogram, choose the medicinal material nearest with the standard medicinal material.Fig. 2 is the collection of illustrative plates of standard medicinal material, and Fig. 3 is a collection of illustrative plates of choosing medicinal material.
B, the ethanol with 90% carry out diacolation.As shown in Figure 4, the diacolation device is a kind of traditional medicinal material extract equipment, and it is a ceramic doline device, and filter sieve and cotton placed thereon are arranged at funnel shaped bottom, needs the medicinal material of diacolation to be positioned on this filter sieve.It is solvent (because ethanol nontoxic, low price) that the present invention selects ethanol, and ethanol ceaselessly drips from suitable for reading, and percolate ceaselessly flows out from end opening, makes to have a concentration gradient in the device, helps the removal of compositions such as saponin(e in the Radix Liriopes.Adopt the ethanol of 6 times of amounts to carry out diacolation, the ethanol consumption can cause the dissolving of sugar too much, and consumption is difficult for again saponin etc. is extracted very little.Mark in the accompanying drawing: 1 is percolating device; 2 is filter sieve; 3 is cotton; 4 is the Radix Liriopes meal; 5 is ethanol; 6 are ethanol stream inlet and control valve; 7 is the percolate spout.
Filter residue behind C, the diacolation extracts 2 times 85 ℃ of water-baths with the water of 10 times of amounts, each 30min.The number of times that extracts has considerable influence to the Radix Liriopes polysaccharide extract rate, so minimum should the repetition extracted once.Extraction time is too much also uneconomical, so be chosen to be 2 times.
D, filtrate are concentrated into 1/10 of original volume after merging, and add 95% ethanol again, and making the ethanol ultimate density is 80% o'clock, and alcohol is analysed; The ultimate density that guarantees alcohol precipitation is 80% very important, and excessive concentration monose etc. is easily separated out, and concentration is crossed low then polysaccharide and separated out incomplete.
After E, alcohol are analysed be deposited in 50 ± 2 ℃ of vacuum-dryings after, beat powder, resulting powder is the Radix Liriopes polyoses extract that is extracted.
The content of Radix Liriopes polysaccharide in F, the usefulness spectrophotometry extract.This is a kind of method of traditional mensuration polysaccharide, can also measure polysaccharide with other analytical procedure.According to the inventor's determination data, the Radix Liriopes polyoses extract can reach 30% of raw medicinal material dry weight, and the content of polysaccharide is generally 73-87% in the extract, reaches as high as 90%.
Claims (5)
1, a kind of extraction process of Radix Liriopes polysaccharide is characterized in that: the extraction process of Radix Liriopes polysaccharide is carried out according to following steps in order:
A, be benchmark, use high performance liquid chromatography-GC-MS, choose piece root with standard medicinal ingredient, Radix Liriopes that content is close according to medicinal materials fingerprint with the control medicinal material of national Nat'l Pharmaceutical ﹠ Biological Products Control Institute;
B, the meal tuber of dwarf lilyturf is cleaned, is prepared as to the Radix Liriopes piece root of choosing, with the Radix Liriopes meal with 5-7 ethanol diacolation in the diacolation device of 90% doubly;
C, the dregs of a decoction go to the alcohol back to extract 2-3 time each 20-40 minute with 8-12 times of water in 70-98 ℃ of water-bath;
D, filtrate merge the back and are evaporated to 1/10 of volume at 60 ℃, add 95% ethanol, and making pure content is 80% o'clock, and alcohol is analysed;
E, with alcohol analyse be deposited in 45-55 ℃ of vacuum-drying after, beat powder, resulting powder is the Radix Liriopes polyoses extract that is extracted.
The content of Radix Liriopes polysaccharide in F, the usefulness spectrophotometry extract.
2, extraction process according to claim 1 is characterized in that: the Radix Liriopes meal is with in the ethanol percolation operation, and consumption of ethanol doubly is good with 5.5-6.5, and the best is 6 times;
3, according to the extraction process described in the claim 1, it is characterized in that: the described dregs of a decoction go in the extracting in water operation of alcohol back, and the consumption of water doubly is good with 9-11, and optimum amount is 10 times; Extracting temperature is good with 75-90 ℃, and optimum temps is 85 ± 2 ℃; The optimum extraction number of times is 2 times; Each extraction time is 30min.
4, extraction process according to claim 1 is characterized in that: described vacuum drying optimum temps is 50 ± 2 ℃.
5, according to the described extraction process of arbitrary claim in the claim 1 to 4, it is characterized in that: instrument such as the liquid chromatography that can also adopt other to choosing of raw material Radix Liriopes, infrared spectra carries out.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021477582A CN1305908C (en) | 2002-11-29 | 2002-11-29 | Extracting technology for mountain ophiopogon root polysaccharide |
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| CNB021477582A CN1305908C (en) | 2002-11-29 | 2002-11-29 | Extracting technology for mountain ophiopogon root polysaccharide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935359A (en) * | 2010-09-10 | 2011-01-05 | 中国药品生物制品检定所 | Liriope muscari baily polysaccharide and preparation method thereof |
| CN101559166B (en) * | 2009-05-26 | 2011-09-21 | 中山大学 | Ophiopogon japonicus extract, preparation method and hypoglycemic application thereof |
| CN102336931A (en) * | 2011-10-25 | 2012-02-01 | 温州医学院 | Ophiopogonpolysaccharide, and preparation method and application thereof |
| CN102391388A (en) * | 2011-12-13 | 2012-03-28 | 云南瑞升烟草技术（集团）有限公司 | Method for extracting polysaccharides of ophiopogon japonicus by subcritical water and application in cigarette |
| CN102757508A (en) * | 2011-04-25 | 2012-10-31 | 上海张江中药现代制剂技术工程研究中心 | Application of ophiopogon polysaccharide extract in preparing foodstuff additives, health-care products or medicines with weight-reducing function |
| CN105997728A (en) * | 2016-07-12 | 2016-10-12 | 曹蕊 | Liriope platyphylla Wang et Tang extract with anti-aging activity and preparation method and application thereof |
| CN109541098A (en) * | 2018-11-27 | 2019-03-29 | 华润三九（雅安）药业有限公司 | Radix Ophiopogonis finger-print, its construction method and Radix Ophiopogonis quality determining method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1069650C (en) * | 1995-12-29 | 2001-08-15 | 中国科学院上海药物研究所 | Method for separation and purification of lentinan |
| CN1100792C (en) * | 2000-05-18 | 2003-02-05 | 厦门中卫多糖研究所 | Longan polysaccharide extracting process |
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2002
- 2002-11-29 CN CNB021477582A patent/CN1305908C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559166B (en) * | 2009-05-26 | 2011-09-21 | 中山大学 | Ophiopogon japonicus extract, preparation method and hypoglycemic application thereof |
| CN101935359A (en) * | 2010-09-10 | 2011-01-05 | 中国药品生物制品检定所 | Liriope muscari baily polysaccharide and preparation method thereof |
| CN102757508A (en) * | 2011-04-25 | 2012-10-31 | 上海张江中药现代制剂技术工程研究中心 | Application of ophiopogon polysaccharide extract in preparing foodstuff additives, health-care products or medicines with weight-reducing function |
| WO2012145946A1 (en) * | 2011-04-25 | 2012-11-01 | 上海张江中药现代制剂技术工程研究中心 | Application of dwarf lilyturf tuber polysaccharide extract in preparation of dietary supplement, health food or medicine with the function of weight loss |
| CN102757508B (en) * | 2011-04-25 | 2015-11-25 | 上海张江中药现代制剂技术工程研究中心 | A kind of Radix Ophiopogonis polysaccharide extract has the application in the foodstuff additive of weight losing function, healthcare products or medicine in preparation |
| CN102336931A (en) * | 2011-10-25 | 2012-02-01 | 温州医学院 | Ophiopogonpolysaccharide, and preparation method and application thereof |
| CN102391388A (en) * | 2011-12-13 | 2012-03-28 | 云南瑞升烟草技术（集团）有限公司 | Method for extracting polysaccharides of ophiopogon japonicus by subcritical water and application in cigarette |
| CN102391388B (en) * | 2011-12-13 | 2014-04-02 | 云南瑞升烟草技术（集团）有限公司 | Method for extracting polysaccharides of ophiopogon japonicus by subcritical water and application in cigarette |
| CN105997728A (en) * | 2016-07-12 | 2016-10-12 | 曹蕊 | Liriope platyphylla Wang et Tang extract with anti-aging activity and preparation method and application thereof |
| CN109541098A (en) * | 2018-11-27 | 2019-03-29 | 华润三九（雅安）药业有限公司 | Radix Ophiopogonis finger-print, its construction method and Radix Ophiopogonis quality determining method |
| CN109541098B (en) * | 2018-11-27 | 2020-11-10 | 华润三九（雅安）药业有限公司 | Radix ophiopogonis fingerprint spectrum, construction method thereof and radix ophiopogonis quality detection method |
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| CN1305908C (en) | 2007-03-21 |
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