CN1156485C - Process for extracting, separating and refining amygdalin - Google Patents
Process for extracting, separating and refining amygdalin Download PDFInfo
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- CN1156485C CN1156485C CNB021004609A CN02100460A CN1156485C CN 1156485 C CN1156485 C CN 1156485C CN B021004609 A CNB021004609 A CN B021004609A CN 02100460 A CN02100460 A CN 02100460A CN 1156485 C CN1156485 C CN 1156485C
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Abstract
The present invention relates to a method for extracting, separating and refining amygdalin as an effective ingredient. Bitter apricot kernels after being taken, squeezed and deoiled are extracted with added ethanol in the quantity 3 to 6 times larger than that of the bitter apricot kernels for 3 times and filtered at reduced pressure; filtered solutions are merged, the ethanol is recovered at reduced pressure to a proper quantity and placed to separate out the amygdalin filtered to obtain a crude amygdalin product. The crude amygdalin product is dissolved with added ethanol, filtered, stored in a refrigerated mode and placed to separate out a white clustered crystal of the amygdalin; the crystal is filtered at reduced pressure, washed with a small quantity of ethyl ether and a small quantity of ethanol and crystallized to obtain a quantitative amygdalin reference substance with the purity higher than 99%. The present invention has the advantages of simple and convenient method, high extraction rate, high purity of the reference substance and wide application values. The crude amygdalin product with the purity of higher than 50% and the quantitative amygdalin reference substance with the purity of higher than 99% can be directly extracted with the ethanol without column chromatography. The present invention solves the long-term problems of destroy of the effective ingredient and curative effect reduction which are caused by the amygdalin easily enzymolyzed or hydrolyzed by emulsin.
Description
Technical field
The present invention relates to a kind of extraction, separation and process for purification of amygdalin.
Background technology
Semen Armeniacae Amarum is the kind that Chinese Pharmacopoeia is gone through version collection, and the cough-relieving of tool sending down abnormally ascending, the effect of relievining asthma, relaxing bowel are used for cough, asthma, fullness sensation in chest, phlegm is many, bloody sputum Tianjin is withered, the dry constipation of intestines, is the medicine of using always clinically.According to the literature, amygdalate cough-relieving effective ingredient mainly is that amygdaloside slowly decomposes in vivo, produces micro-prussic acid gradually and suppresses respiratory centre, makes respiratory movement be tending towards quiet and presents the antitussive and antiasthmatic effect.Semen Armeniacae Amarum and degradation production thereof also have sedative effect etc. in addition.
But the preparation so that the Semen Armeniacae Amarum crude drug adds often owing to enzymolysis, is difficult to detect amygdaloside.And in the preparation that extracts processing, present amygdaloside extraction process mostly is poach and carries general extractive or steam distillation, because amygdaloside is heated and very easily destroyed in water for a long time, its content is all lower, be difficult to measure content, even be difficult to qualitative detecting.
Summary of the invention
Technical problem to be solved by this invention provides a kind of extraction yield height, quantitatively extraction, separation and the process for purification of reference substance purity height, amygdalin that method is easy.
The technical solution adopted for the present invention to solve the technical problems is: get Semen Armeniacae Amarum, after squeezing is deoiled, add the extraction using alcohol 3 times of 3～6 times of amounts, filtration under diminished pressure, merging filtrate, decompression recycling ethanol is to an amount of, place, separate out amygdaloside, filter the amygdaloside crude product.
A small bundle of straw, etc. for silkworms to spin cocoons on shape crystallization of amygdaloside white is placed, separated out to its treating process for the amygdaloside crude product is added dissolve with ethanol, filtration, refrigeration, filtration under diminished pressure, with a small amount of ether and washing with alcohol crystallization, purity is the quantitative reference substance of amygdaloside more than 99%.
Principle of the present invention is as follows:
According to the amygdaloside facile hydrolysis with by synaptase enzymolysis destructive character, selected for use Semen Armeniacae Amarum squeezing deoiled after, the method with alcohol reflux has reduced destruction, fast, obtains through refining amygdaloside crude product and quantitative reference substance simply.
Beneficial effect of the present invention is as follows:
(1) the invention provides a kind ofly, directly use extraction, separation, the method for refining of the quantitative reference substance of extraction using alcohol amygdaloside without column chromatography.Semen Armeniacae Amarum cake after the amygdaloside crude product that extracts deoils for squeezing, extraction yield can reach more than 8%, and the content of amygdaloside can reach more than 50%.The quantitative reference substance content of amygdaloside can reach more than 99%.
(2) amygdaloside that the present invention obtained through refining can directly add in the preparation, has solved for a long time because amygdaloside, makes the difficult problem that effective ingredient is destroyed, curative effect reduces easily by synaptase enzymolysis or hydrolysis.Amygdalate effective ingredient is fully used, has guaranteed curative effect, reduced taking dose.
(3) amygdaloside obtained through refining of the present invention regularly the purity of reference substance reach 99.2%, can compare product use for medical research, production unit, tool is the effect of using value and the promotion modernization of Chinese medicine widely.
(4) mere formality is offered report, amygdaloside tool antitumous effect, and the amygdaloside that the present invention obtained through refining provides basic substance for the development of cancer therapy drug.
(5) the present invention directly uses the solvent extraction amygdaloside without column chromatography, and turnout is unrestricted, can obtain through refining the amygdaloside monomer in a large number, for production application.
Description of drawings
Discriminating amygdaloside purity test (HPLC normalization method) color atlas that Fig. 1 provides for Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Fig. 2 is quantitative with amygdaloside reference substance purity test (NPLC normalization method) color atlas for what the present invention produced.
Embodiment
Embodiment 1:
The Semen Armeniacae Amarum cake 1.5kg after deoiling is pressed in pressure, coarse crushing, add ethanol 4.5～9kg, refluxing extraction 3 times, suction filtration while hot, merging filtrate, decompression recycling ethanol refrigerates, places, separates out amygdaloside to an amount of, suction filtration, the dry amygdaloside crude product 120g that gets, yield is 8%, measures that amygdaloside content is 60% in the amygdaloside crude product.
Get amygdaloside crude product 5g again, add bunch shape crystallization that dissolve with ethanol, filtration, refrigeration are placed, separated out Semen Armeniacae Amarum white, filtration under diminished pressure, with a small amount of ether and washing with alcohol crystallization, aforesaid operations is 1～2 time repeatedly, must the quantitative reference substance 1.5～2.5g of amygdaloside.Fusing point is 214.8～216.5 ℃, and surveying its purity with high performance liquid phase normalization method is 99.2%.
The affirmation of the quantitative reference substance of institute's purified amygdaloside of the present invention and the detection of purity and content thereof:
One, the affirmation of the quantitative reference substance of amygdaloside:
1, crystalline form: the quantitative reference substance of the amygdaloside that the present invention obtains through refining is white bunch plate crystal.
2, fusing point: get the quantitative reference substance of amygdaloside that the present invention obtains through refining, dry, porphyrize, the dress kapillary is measured its fusing point with YRT-3 fusing point instrument, measures three times, is respectively:
①215.4～216.5℃；②214.8～216℃；③215～216℃
Its fusing point is: 214.8～216.5 ℃.
According to the literature: amygdaloside trihydrate fusing point is 200 ℃, and the anhydride fusing point is 220 ℃.
3, thin-layer chromatography: the amygdaloside that getting Nat'l Pharmaceutical ﹠ Biological Products Control Institute (inspection institute in abbreviating as) provides is differentiated reference substance (lot number: 820-9401) add 50% methyl alcohol and be mixed with the solution that 1ml contains 2mg, in contrast product solution.Get the amygdaloside that the present invention obtains through refining again, add 50% methyl alcohol and be mixed with the solution that every 1ml contains 2mg, as need testing solution.Draw above-mentioned two kinds of each 10ul of solution respectively, put respectively in same be on the silicic acid GF254 thin layer plate of tackiness agent with the Xylo-Mucine, upper solution with propyl carbinol-Glacial acetic acid-water (6: 1: 3) is a developping agent, launch, take out, dry, put under the ultra-violet lamp (UV254nm) and inspect, in the trial-product chromatogram, with the corresponding position of reference substance chromatogram on show the spot of same color.After spraying 5% phospho-molybdic acid anhydrous alcohol solution, spray 10% sulfuric acid ethanol liquid again, about 10 minutes of 100 ℃ of bakings, spot colour developing is clear, in the trial-product chromatogram with the corresponding position of reference substance chromatogram on show the same color spot.
4, HPLC chromatogram:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is weighting agent;
Fine-0.25% the phosphoric acid solution of second (1: 67) is a moving phase; The detection wavelength is 210nm; Flow velocity 0.91ml/min, theoretical plate number is calculated by amygdaloside should be not less than 5000.
The amygdaloside that inspection is provided in getting is differentiated reference substance, adds 50% methyl alcohol and makes the solution that every 1ml contains 0.04mg, in contrast product solution.Get the present invention again and make the quantitative reference substance of amygdaloside and add 50% methyl alcohol and make every 1ml and contain 0.04mg solution, as need testing solution.
Press Chinese Pharmacopoeia version appendix in 2000 high-efficient liquid phase technique, inject 20ul respectively, reference substance is consistent with the liquid chromatogram retention time of trial-product (differentiating amygdaloside and amygdaloside of the present invention).
More than 4 experiment conclusive evidences, the discriminating amygdaloside reference substance that amygdaloside that the present invention obtains through refining and middle inspection are provided is same compound.
Two, purity and content:
Still differentiate that with the amygdaloside that middle inspection was provided reference substance is contrast, adopt the normalization method of high-efficient liquid phase technique to carry out purity and content inspection.The reference substance that middle inspection is provided also has a small peak to occur before the main peak of amygdaloside, and the amygdaloside reference substance that the present invention obtains through refining then inclusion-free peak occurs.The inspection reference substance content of differentiating was 97.2% during the normalization method recorded, and the quantitative reference substance of the amygdaloside that the present invention obtains through refining is 99.2% (seeing Fig. 1-2).
Claims (2)
1, a kind of extraction of amygdalin, separation and process for purification is characterized in that getting Semen Armeniacae Amarum, after squeezing is deoiled, the extraction using alcohol 3 times that adds 3～6 times of amounts, filtration under diminished pressure, merging filtrate, amygdaloside is placed, separated out to decompression recycling ethanol to an amount of, filter the amygdaloside crude product.
2, the extraction of amygdalin according to claim 1, separation and process for purification, it is characterized in that the amygdaloside crude product is added dissolve with ethanol, filtration, refrigeration, a small bundle of straw, etc. for silkworms to spin cocoons on shape crystallization of place, separating out amygdaloside white, filtration under diminished pressure, with a small amount of ether and washing with alcohol crystallization, purity is the quantitative reference substance of amygdaloside more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021004609A CN1156485C (en) | 2002-02-01 | 2002-02-01 | Process for extracting, separating and refining amygdalin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021004609A CN1156485C (en) | 2002-02-01 | 2002-02-01 | Process for extracting, separating and refining amygdalin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1365979A CN1365979A (en) | 2002-08-28 |
| CN1156485C true CN1156485C (en) | 2004-07-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021004609A Expired - Fee Related CN1156485C (en) | 2002-02-01 | 2002-02-01 | Process for extracting, separating and refining amygdalin |
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| CN (1) | CN1156485C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100470294B1 (en) * | 2002-08-20 | 2005-02-05 | (주) 한약마을 | Extraction method for effectively obtaining amygdalin from Persicae Semen and Armenicae Semen |
| CN1318439C (en) * | 2003-12-24 | 2007-05-30 | 天津市南开医院 | Preparation method of amygdalin and its application in preparation of amygdalin preparation for promoting the blood circulation of heart, brain, pancreas and wound |
| CN101558795B (en) * | 2008-11-07 | 2012-06-27 | 中国农业大学 | Method for reducing residual fat of almond cakes by dipping and pressing |
| CN102234298A (en) * | 2010-04-23 | 2011-11-09 | 华东理工大学 | Method for extracting and purifying amygdalin from peach seeds |
| CN102174071A (en) * | 2011-01-06 | 2011-09-07 | 西北农林科技大学 | Method for extracting and preparing protein powder and enzymolysis product thereof from almond meal |
| CN102702282B (en) * | 2012-06-04 | 2014-11-26 | 西安天丰生物科技有限公司 | Method for separating amygdalin from almond oil residue |
| CN105748644A (en) * | 2014-12-19 | 2016-07-13 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Traditional Chinese medicine composition with effects of stopping cough and relieving asthma and preparation method of traditional Chinese medicine composition |
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2002
- 2002-02-01 CN CNB021004609A patent/CN1156485C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1365979A (en) | 2002-08-28 |
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