CN1962682A - American waerplantain triterpenoidal alcohol extract and its preparation method - Google Patents
American waerplantain triterpenoidal alcohol extract and its preparation method Download PDFInfo
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- CN1962682A CN1962682A CN 200610154797 CN200610154797A CN1962682A CN 1962682 A CN1962682 A CN 1962682A CN 200610154797 CN200610154797 CN 200610154797 CN 200610154797 A CN200610154797 A CN 200610154797A CN 1962682 A CN1962682 A CN 1962682A
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Abstract
The invention discloses an Alismatale triterpenoidal alcohol extract and preparing method with not less than 60% acetate, which comprises the following steps: adopting normal alcohol solution to extract Alismatale; refining to obtain the Alismatale triterpenoidal alcohol extract; improving effective component.
Description
Technical field
The present invention relates to a kind of American waerplantain triterpenoidal alcohol extract and preparation method thereof.
Technical background
Rhizoma alismatis is the dry tuber of Alismataceae plant rhizoma alismatis Alisma orientalis (Sam.) Juzep..The contained total triterpene alcohols of rhizoma alismatis is the main active ingredient of its reducing blood-fat pharmacology effect.Existing extracting method is with alcohol or other organic solvents, and supercritical extraction extracts the relevant medicinal ingredients of rhizoma alismatis.Method is:
1, rhizoma alismatis powder (crossing 20 mesh sieves) is used 90% alcohol reflux, reclaims ethanol, gets medicinal extract, and yield is about 6%.With macroporous resin on the medicinal extract (AB-8) post, with water, 40% ethanol, 95% ethanol elution, yield is respectively 27.4%, 5.7%, 34.9% respectively.95% ethanol elution position is the refining thing of rhizoma alismatis macroporous resin.In rhizoma alismatis B monoacetate, its total triterpene alcohol content is 10%.American waerplantain triterpenoidal alcohol content is very low in the Rhizoma Alismatis extract of method 1 system, and unfavorable pharmacy is used;
2, get rhizoma alismatis powder (crossing 60 mesh sieves), the supercritical CO of packing into
2Extractor, adjusting extracting pressure are that 26MPa, temperature are that 50 ℃, CO2 flow are 20-23Kg/h, extraction 1.5h, extract, yield is about 1.5%, in rhizoma alismatis B monoacetate, its total triterpene alcohol content is about 55%.The content that method 2 is got only triterpene alcohol in the rhizoma alismatis extraction compares higher, but also there is certain problem in technology: supercritical extraction need under high pressure carry out (26MPa), to equipment requirements than higher, the industrialized production cost is higher, be not easy extensive the use and produce, also have the yield of the American waerplantain triterpenoidal alcohol extract that method 2 obtains lower.
Summary of the invention
The object of the present invention is to provide a kind of American waerplantain triterpenoidal alcohol extract, wherein contain the American waerplantain triterpenoidal alkylol cpd and be no less than 60% in Alisol B std 23-acetic ester, be preferably 60-90%, 70-80% most preferably, this extract has improved the content of the total triterpene alcohol compound of American waerplantain triterpenoidal alcohol extract of existing record.
The present invention also aims to provide the preparation method of the higher Rhizoma Alismatis extract of a kind of triterpene alcohol compound content, this method comprises extraction, treating process, active constituent content height in the Rhizoma Alismatis extract that this method obtains, the extract behind the refining purifying more helps its application in pharmacy.The content of Rhizoma Alismatis extract of the present invention is higher, reducing taking dose when medicinal, and obtaining the content of American waerplantain triterpenoidal alcohol extract, existing technology such as method 1 have only 10%, content is very low, bigger at dosage when medicinal, dosing a patient with makes troubles.
The preparation method of above-mentioned Rhizoma Alismatis extract provided by the invention, comprising with the alcohol of rhizoma alismatis medicinal material or acetone extract with solvent method or (with) column chromatography makes with extra care, with the process of the extract of total triterpene alcohol compound of obtaining high level.
The invention provides a kind of method for preparing American waerplantain triterpenoidal alcohol extract, may further comprise the steps:
1) extract: with lower alcohol, acetone or both mixing solutionss or contain the above-mentioned organic solvent extraction that content is lower than 40% water, and reflux, the temperature of reflux is 70-100 ℃;
2) concentrated or dry: concentrating under reduced pressure or constant pressure and dry extracting solution are to thick;
3) refining: the extract that step 2 is obtained is directly gone up macroporous adsorptive resins or is suspended in water earlier, uses the middle polarity organic solvent extraction, goes up macroporous adsorptive resins behind the evaporate to dryness again; With lower concentration alcohol or the removal of impurities of aqueous acetone solution wash-out, with the alcoholic solution or the acetone water elution of high density, collect elutriant again, concentrating under reduced pressure, constant pressure and dry or spraying drying promptly get American waerplantain triterpenoidal alcohol extract.
Wherein the described lower alcohol of step 1 is one or more any mixing in methyl alcohol, ethanol or the propyl alcohol; Macroporous adsorbent resin filler model in the step 3 is D101 or D001; Applied sample amount is counted 1:6-14, preferred 1:8-12 with filler and the weight ratio that is converted between the extract of crude drug amount; Extraction solvent is any in chloroform or methylene dichloride, tetracol phenixin, ethyl acetate or the ether, a kind of in preferred methylene dichloride or the ethyl acetate; The lower concentration alcoholic solution is 35-55%, preferred 45-50%; The high density alcoholic solution is characterized as 80-95%, preferred 85-90%.
The concrete grammar of the total triterpene alcohol compound of extraction rhizoma alismatis provided by the invention is:
(1) with rhizoma alismatis pulverizing medicinal materials (about 20 order), with lower alcohol such as methyl alcohol or ethanol or propyl alcohol, acetone or aqueous lower alcohol, the acetone refluxing extraction, the aqueous ethanolic solution of wherein preferred 60-95%, 80% aqueous ethanolic solution most preferably, the solvent add-on is that the 8-10 of medicinal material doubly measures, wherein preferred 8 times of amounts, refluxing extraction 1-4 hour, wherein preferred 2 hours, filter, the dregs of a decoction repeat to extract twice by above-mentioned condition, united extraction liquid concentrates and is recycled to 1/4 volume, and low temperature was placed 12 hours, filtration or centrifugal, supernatant liquor reclaims concentrating under reduced pressure and is recycled to 1/3 volume (proportion is 1.08).Extract the middle polarity organic solvent extraction such as the chloroform of gained will be concentrated, methylene dichloride, tetracol phenixin, ethyl acetate or ether) extraction, preferred methylene dichloride, ethyl acetate is as extraction agent, the volume of methylene dichloride is that the 0.2-0.5 of the aqueous solution doubly measures, wherein preferred 0.3 times, extract 5-6 time, after the extraction liquid that obtains reclaims methylene dichloride, last macroporous resin (D001 or D101) column chromatography, after extracting solution added resin column, earlier remove impurity with 35-55% lower alcohol or aqueous acetone solution wash-out, wherein preferred 50% aqueous ethanolic solution wash-out, the elute soln amount is about 3 times of retention volume, this wash-out partly discards not, use 80-95% lower alcohol or aqueous acetone solution wash-out again, wherein preferred 90% aqueous ethanolic solution is collected elutriant, the elute soln amount is 3-5 a times of retention volume, merge elutriant concentrating under reduced pressure or spraying and be the total triterpenoidal alcohol extract of rhizoma alismatis of the present invention, yield is about 2.5%, the product of different batches is the standard substance spectrophotometry with Alisol B std 23-acetic ester, and content is 73-75%.
(2) with rhizoma alismatis pulverizing medicinal materials (about 20 orders), with lower alcohol, acetone or aqueous lower alcohol, acetone refluxing extraction, the aqueous ethanolic solution of wherein preferred 70-95%, 80% aqueous ethanolic solution most preferably, the volume add-on is that the 8-10 of medicinal material doubly measures, wherein preferred 8 times of amounts, refluxing extraction 1-4 hour, wherein preferred 2 hours, filter, the dregs of a decoction repeat to extract twice by above-mentioned condition, united extraction liquid is recycled to 1/4 volume, and low temperature was placed 12 hours, filter (or centrifugal), supernatant liquor reclaims about 1/3 (proportion is 1.07) of decompression original volume.Said extracted liquid can be directly used in macroporous resin column chromatography, chromatographic stuffing can be selected macroporous adsorbent resin such as D001 or D101 resin for use, after extracting solution added resin column, earlier remove impurity with 35-55% lower alcohol or aqueous acetone solution wash-out, wherein preferred 50% aqueous ethanolic solution wash-out, the elute soln amount is about 3 times of retention volume, this wash-out partly discards not, use 80-95% lower alcohol or aqueous acetone solution wash-out again, wherein preferred 90% aqueous ethanolic solution is collected elutriant, the elute soln amount is 3-5 a times of retention volume, merge elutriant concentrating under reduced pressure or spraying drying and promptly get American waerplantain triterpenoidal alcohol extract, yield is about 3.2%, and the product of different batches is the standard substance spectrophotometry with Alisol B std 23-acetic ester, and content is 60-65%.
The method that the present invention adopts macroporous adsorbent resin (D001 or D101) purifying or methylene dichloride (ethyl acetate) extraction and macroporous adsorbent resin (D001 or D101) purifying to combine is made with extra care crude extract, thereby obtains high-load American waerplantain triterpenoidal alcohol extract of the present invention.The present invention can also pass through to repeat macroporous resin adsorption chromatography (D001 or D101) process, thereby improves the content of triterpene alcohol in the American waerplantain triterpenoidal alcohol extract.
Content assaying method:
1, sample solution preparation: it is an amount of to get the American waerplantain triterpenoidal alcohol efficient part, and 65 ℃ to revolve evaporate to dryness dry, must contain the less medicinal extract of moisture, and precision takes by weighing 17.89mg, and the analytical pure dissolve with methanol is fixed molten to 50ml, promptly.
2, standard solution preparation: precision takes by weighing Alisol B std 23-acetic ester (〉=96%) 9.0mg, and the analytical pure dissolve with methanol is fixed molten to 50ml, promptly.
2, measuring method:
The typical curve preparation: 1) maximum absorption wavelength is determined: Alisol B std 23-acetate solution 400-700nm scanning gets λ max=570nm.
2) liquid preparation to be measured: precision is measured standard solution 0.0,0.2,0.3,0.4,0.5,0.6ml puts dried sanitary equipment plug in vitro, volatilizes methyl alcohol in boiling water bath; Add 1.0ml 8% Vanillin ethanol solution, shake up; Add 5.0ml 77% sulphuric acid soln, shake up; 60 ℃ of heating in water bath 10 minutes, ice-water bath 15 minutes, room temperature 10 minutes.
3) λ max=570nm place measures light absorption value A, the drawing standard curve, and regression equation is: y=0.0351
*X, relation conefficient is 0.9992;
4) precision is measured sample solution 0.2,0.3,0.4ml, and operation in accordance with the law gets light absorption value A, gets the corresponding content value of its mean value calculation promptly.
Preparation method of the present invention has following technical superiority: 1, compares with extraction using alcohol AB8 resin purification technology, and the content height (more than 55%) of total triterpene alcohol in the American waerplantain triterpenoidal alcohol extract that the inventive method makes, and former method content instrument has about 10%.
2, compare with supercritical extraction process, the extraction that preparation method of the present invention adopted, the method for macroporous resin column chromatography are many at present can be used for industrial production on a large scale, and required equipment is simple, and equipment cost is low; And (running cost is low for D-101, D-001) renewable use, and liquid C02 loss is bigger for institute of the present invention macroporous resin filler; The yield height of the American waerplantain triterpenoidal alcohol extract that the inventive method prepares (yield＞2.5%, and supercritical extraction process is 1.5%.)
Embodiment
Following examples are in order further to describe the present invention for example, rather than limit the present invention by any way.
Embodiment 1: the preparation method I of the total triterpenoidal alcohol extract of rhizoma alismatis
With rhizoma alismatis pulverizing medicinal materials (about 20 orders), aqueous ethanolic solution with 80%, the solvent add-on is 8 times of amounts of medicinal material, and refluxing extraction 2 hours is filtered, the dregs of a decoction repeat to extract twice by above-mentioned condition, united extraction liquid is recycled to 1/4 volume, and low temperature was placed 12 hours, filter (or centrifugal), supernatant liquor reclaims 1/3 (proportion is 1.07) of decompression original volume.Said extracted liquid is directly used in macroporous resin column chromatography, chromatographic stuffing is the D101 resin, after extracting solution added resin column (going up the sample ratio is 1: 12), earlier with 50% aqueous ethanolic solution wash-out, the elute soln amount is about 3 times of retention volume, this wash-out partly discards not, collect elutriant with 90% aqueous ethanolic solution again, the elute soln amount is 3-5 a times of retention volume, merge elutriant concentrating under reduced pressure or spraying drying and promptly get total triterpene alcohol compound extract, yield is about 3.2%, and the product of different batches is the standard substance spectrophotometry with Alisol B std 23-acetic ester, and content is 60-65%.
Embodiment 2: the preparation method II of the total triterpenoidal alcohol extract of rhizoma alismatis
With rhizoma alismatis pulverizing medicinal materials (about 20 orders), aqueous ethanolic solution with 80%, the solvent add-on is 8 times of amounts of medicinal material, refluxing extraction 1-4 hour, and wherein preferred 2 hours, filter, the dregs of a decoction repeat to extract twice by above-mentioned condition, united extraction liquid, and low temperature was placed 12 hours, filter (or centrifugal), supernatant liquor reclaims concentrating under reduced pressure and is recycled to 1/4 volume (proportion is 1.08).The extract dichloromethane extraction of gained will be concentrated, the volume of methylene dichloride is 0.3 times of amount of the aqueous solution, extract 5-6 time, after the extraction liquid that obtains reclaims methylene dichloride, last macroporous resin (D001) column chromatography, after extracting solution added resin column (going up the sample ratio is 1: 8), elder generation removes assorted with 50% ethanol aqueous wash, the elute soln amount is about 3 times of retention volume, this wash-out partly discards not, use 90% aqueous ethanolic solution wash-out again, collect elutriant, the elute soln amount is 3-5 a times of retention volume, merge elutriant concentrating under reduced pressure or spraying and be the total triterpenoidal alcohol extract of rhizoma alismatis of the present invention, yield is about 2.5%, and the product of different batches is the standard substance spectrophotometry with Alisol B std 23-acetic ester, and content is 73-75%.
Embodiment 3: the preparation method III of the total triterpenoidal alcohol extract of rhizoma alismatis
With rhizoma alismatis pulverizing medicinal materials (about 20 orders), aqueous ethanolic solution with 80%, the solvent add-on is 8 times of amounts of medicinal material, refluxing extraction 1-4 hour, and wherein preferred 2 hours, filter, the dregs of a decoction repeat to extract twice by above-mentioned condition, united extraction liquid, and low temperature was placed 12 hours, filter (or centrifugal), supernatant liquor reclaims concentrating under reduced pressure and is recycled to 1/4 volume (proportion is 1.07).The extract dichloromethane extraction of gained will be concentrated, the volume of methylene dichloride is 0.3 times of amount of the aqueous solution, extract 5-6 time, after the extraction liquid that obtains reclaims methylene dichloride, last macroporous resin (D101) column chromatography, after extracting solution added resin column (going up the sample ratio is 1: 10), elder generation removes assorted with 50% ethanol aqueous wash, the elute soln amount is about 3 times of retention volume, this wash-out partly discards not, use 90% aqueous ethanolic solution wash-out again, collect elutriant, the elute soln amount is 3-5 a times of retention volume, merge elutriant concentrating under reduced pressure or spraying and be the total triterpenoidal alcohol extract of rhizoma alismatis of the present invention, yield is about 2.5%, and the product of different batches is the standard substance spectrophotometry with Alisol B std 23-acetic ester, and content is 73-75%.
Claims (5)
1. an American waerplantain triterpenoidal alcohol effective part extract that obtains from the rhizoma alismatis extraction is characterized in that triterpene alcohol compound content is at least 60% in Alisol B std 23-acetic ester in the place near the steps extract.
2. extract as claimed in claim 1 is characterized in that described total triterpene alcohol compound content counts 60-90% with Alisol B std 23-acetic ester;
3. method for preparing extract as claimed in claim 1 may further comprise the steps:
1) extract: with lower alcohol, acetone or both mixing solutionss or contain the above-mentioned organic solvent extraction that content is lower than 40% water, and reflux, the temperature of reflux is 70-100 ℃;
2) concentrated or dry: concentrating under reduced pressure or constant pressure and dry extracting solution are to thick;
3) refining: the extract that step 2 is obtained is directly gone up macroporous adsorptive resins or is suspended in water earlier, uses the middle polarity organic solvent extraction, goes up macroporous adsorptive resins behind the evaporate to dryness again; With lower concentration alcohol or the removal of impurities of aqueous acetone solution wash-out, with the alcoholic solution or the acetone water elution of high density, collect elutriant again, concentrating under reduced pressure, constant pressure and dry or spraying drying promptly get American waerplantain triterpenoidal alcohol extract.
4. preparation method as claimed in claim 3 is characterized in that the macroporous adsorbent resin filler model in the described step 3 is D101 or D001; Applied sample amount counts 1 with filler and the weight ratio that is converted between the extract of crude drug amount: the 6-14 extraction solvent is any in chloroform or methylene dichloride, tetracol phenixin, ethyl acetate or the ether, the lower concentration alcoholic solution is 35-55%, and the high density alcoholic solution is characterized as 80-95%.
5. preparation method as claimed in claim 4, applied sample amount preferably counts 1 with filler and the weight ratio that is converted between the extract of crude drug amount: 8-12; Preferred methylene dichloride of extraction solvent or ethyl acetate, the lower concentration alcoholic solution is preferably 45-50%, and the high density alcoholic solution is preferably 85-90%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093454A (en) * | 2010-11-23 | 2011-06-15 | 苏州派腾生物医药科技有限公司 | Preparation method of alisol C monoacetic ester |
| CN102432659A (en) * | 2011-12-15 | 2012-05-02 | 成都普思生物科技有限公司 | Separation and purification method of alisol B 23-acetate monomer |
| CN110314122A (en) * | 2018-03-30 | 2019-10-11 | 深圳市前海博斐生物科技有限公司 | A kind of Alisma extract and its preparation method and application |
-
2006
- 2006-11-27 CN CN 200610154797 patent/CN1962682A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093454A (en) * | 2010-11-23 | 2011-06-15 | 苏州派腾生物医药科技有限公司 | Preparation method of alisol C monoacetic ester |
| CN102093454B (en) * | 2010-11-23 | 2012-08-15 | 苏州派腾生物医药科技有限公司 | Preparation method of alisol C monoacetic ester |
| CN102432659A (en) * | 2011-12-15 | 2012-05-02 | 成都普思生物科技有限公司 | Separation and purification method of alisol B 23-acetate monomer |
| CN110314122A (en) * | 2018-03-30 | 2019-10-11 | 深圳市前海博斐生物科技有限公司 | A kind of Alisma extract and its preparation method and application |
| CN110314122B (en) * | 2018-03-30 | 2023-04-07 | 广州箴美科技有限公司 | Alisma extract and preparation method and application thereof |
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Open date: 20070516 |