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Method for extracting and purifying sequoyitol

A technology of taxol and yew, applied in the field of traditional Chinese medicine extraction, can solve the problems of low yield and the like

Inactive Publication Date: 2007-07-11
SHANGHAI BAILING PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, strictly speaking, the invention of China Pharmaceutical University mainly refers to a mixture rather than a single component; in addition, 60% of the content in the patent of China Pharmaceutical University refers to myo-inositol derivatives The total content is more than 60%, and its yield is very low

Method used

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  • Method for extracting and purifying sequoyitol
  • Method for extracting and purifying sequoyitol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 200 kg of fresh branches and leaves of Taxus chinensis, extract 3 times with 2.5 times the volume of 80% methanol for 3 hours, combine the extracts, concentrate to a viscous solution, add 1:1 (volume / volume) silica gel, stir evenly, Vacuum-dried, crushed, and made into dry samples of raw materials. Pack the column according to the ratio of material: silica gel = 1:20, and load the sample. Gradient eluting with methanol: acetone = 15: 85 and methanol: acetone = 40: 60, the segments were detected by HPLC, the product segments were combined, and concentrated to dryness. Crystallize with absolute ethanol for 3 times, filter and dry to obtain 124.1 g of white crystal powder, which is detected by HPLC method, wherein the content of paclitaxel is 99.68%.

Embodiment 2

[0036] Take 200 kg of dry branches and leaves of Taxus berry, extract 3 times with 2.5 times the volume of 95% ethanol at 50° C. for 3 hours at reflux, combine the extracts, and concentrate until it cannot be concentrated. Dissolve completely with mobile phase methanol: water = 70: 30, put on an acidic macroporous resin chromatography column, use methanol: water = 70: 30-50 as mobile phase gradient elution, monitor by HPLC method, combine the fractions of paclitaxel, Concentrate to dryness under reduced pressure, and crystallize with acetone for 3 times to obtain 212.5 g of white crystalline powder, which is detected by HPLC method, wherein the content of paclitaxel is 99.98%.

Embodiment 3

[0038] Take 2 kg of dry bark powder of Pacific yew, extract 3 times with 2.5 times the amount of 80% acetonitrile at 45° C. for 3 hours under reflux, combine the extracts, and concentrate until it cannot be concentrated. Completely dissolve with mobile phase methanol: water = 70: 30, put on activated carbon chromatography column, use methanol: water = 70: 30 ~ 60 as mobile phase gradient elution, monitor by HPLC method, combine fractions of paclitaxel, concentrate under reduced pressure To dryness, crystallized 3 times with methanol to obtain 1.64 g of white crystalline powder, detected by HPLC method, wherein the content of paclitaxel was 99.12%.

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Abstract

The invention discloses an extracting and purifying method of sequoia alcohol, which comprises the following steps: 1. extracting effective component in the sequoia based on alcohol, acetone or water as extract; obtaining rough raw material with 0.3-5%(wt) sequoia alcohol; 2. adopting rough raw material of sequoia alcohol as raw material to separate through chromatographic system; obtaining the raw material with over 10% sequoia alcohol; 3. crystallizing the sequoia alcohol for 2-4 times; obtaining pure sequoia alcohol with purity over 99%.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicine extraction, in particular to a method for extracting and purifying paclitaxel. Background technique [0002] Sequoyitol is a natural organic compound isolated from yew, which can be used to treat diabetes and other indications. Its molecular formula is as follows: [0003] [0004] Taxol, cephalomannine, 10-DAB III and other important organic substances can be extracted from Taxus chinensis, and docetaxel can be semi-synthesized using 10-DAB III. Among them, paclitaxel and docetaxel are internationally recognized as one of the most effective anticancer drugs. my country's research on the anti-tumor effect of paclitaxel, one of the active ingredients of yew, began in 1984. In 1986, it was included in the "Seventh Five-Year Plan" scientific research plan of the State Administration of Medicine. In February 1995, it was approved by the Ministry of Health to conduct clinical research o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/34C07C43/196
Inventor 杨继东詹华杏林复兴林炯明杨海鹰沈鑫
Owner SHANGHAI BAILING PHARMA TECH CO LTD