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Preparation method of high-content sesquiterpenoids tripterygium alkaloid

A technology of Tripterygium wilfordii alkaloids and sesquiterpenoids, which is applied in the field of medicine, can solve the problems of unfavorable pharmacological research of tripterygium wilfordii sesquiterpenoids alkaloids and difficult to meet the purity, and achieve the effect of low cost and easy operation

Inactive Publication Date: 2011-02-16
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of Tripterygium wilfordii alkaloid monomer mainly adopts liquid / liquid extraction method combined with column chromatography (Lin Sui, Li Yuanchao, Sakurai Nobuko, Guo Shunmin, Deng Fuxiao. Research on Tripterygium wilfordii sesquiterpene alkaloids, Acta Botany, 2001 , 43(6): 647-649; Chen Junyuan, Xia Zhilin, Deng Fuxiao. Improvement of the extraction process of tripterygium wilfordii alkaloids, Chinese Journal of Pharmaceutical Industry, 1989, 20(11): 484-485) and high-speed countercurrent chromatography (High-speed countercurrent chromatography, HSCCC) (CN100422188C), etc., mainly use the rhizome of Tripterygium wilfordii as raw material, and the obtained tripterygium alkaloid monomer content is generally about 95% or lower, and its purity is difficult to meet the medical comparison of tripterygium wilfordii alkaloid monomer It is not conducive to further research on the pharmacology of Sesquiterpene alkaloids of Tripterygium wilfordii

Method used

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  • Preparation method of high-content sesquiterpenoids tripterygium alkaloid
  • Preparation method of high-content sesquiterpenoids tripterygium alkaloid
  • Preparation method of high-content sesquiterpenoids tripterygium alkaloid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 5.0g of triptolide and triptolide ethyl acetate extract waste liquid from which triptolide and triptolide have been removed, evaporate the solvent, weigh 2.0g in a beaker, extract with 10mL chloroform each time, repeat 3 times , combined the chloroform layers, and evaporated to dry to obtain the chloroform extract; then the chloroform extract was extracted 3 times with 10g / L acetic acid, the acetic acid extract was combined, and the pH was adjusted to 10 with 10g / L ammonia water, and the precipitate was filtered with deionized Wash with water for 5 times and dry to obtain crude total alkaloids, then add 30.0 mL of methanol to dissolve, carry out recrystallization at room temperature, and use the raw materials obtained by recrystallization for chromatographic separation.

[0025] The crude total alkaloids of Tripterygium wilfordii obtained by recrystallization were dissolved in a mixed solvent of acetonitrile and water with a volume ratio of 60:40, and then a mixture...

Embodiment 2

[0027] Take 5.0g of triptolide and triptolide ethyl acetate extract waste liquid from which triptolide and triptolide have been removed, evaporate the solvent, weigh 2.0g in a beaker, extract with 10mL chloroform each time, repeat 3 times , combined the chloroform layers, and evaporated to dry to obtain the chloroform extract; then the chloroform extract was extracted 3 times with 10g / L formic acid, the formic acid extract was combined, and the pH was adjusted to 6 with 15g / L formic acid ammonia water, and the precipitate was filtered and used Wash 5 times with deionized water and dry to obtain crude total alkaloids, then add 20.0 mL of isopropanol to dissolve, carry out recrystallization at room temperature, and use the raw materials obtained by recrystallization for chromatographic separation.

[0028] The crude total alkaloids of Tripterygium wilfordii obtained by recrystallization were dissolved in a mixed solvent of acetonitrile and water with a volume ratio of 99:1, and t...

Embodiment 3

[0030] Take 10.0g of triptolide and triptolide ethyl acetate extract waste liquid from which triptolide and triptolide have been removed, evaporate the solvent, weigh 2.0g in a beaker, extract with 10mL chloroform each time, repeat 3 times , combined the chloroform layers, and evaporated to dry to obtain the chloroform extract; then the chloroform extract was extracted 3 times with 10g / L acetic acid, the acetic acid extract was combined, and the pH was adjusted to 10 with 8g / L ammonia water, and the precipitate was filtered with deionized Wash with water for 5 times and dry to obtain crude total alkaloids, then add 10.0-50.0mL of methanol to dissolve, carry out recrystallization at room temperature, and use the raw materials obtained by recrystallization for chromatographic separation.

[0031] The crude total alkaloids of Tripterygium wilfordii obtained by recrystallization are dissolved in a mixed solvent of acetonitrile and water with a volume ratio of 75:25, and the mixture...

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Abstract

The invention discloses a method of separately preparing high-content sesquiterpenoids tripterygium alkaloid monomers by using semi-preparation chromatography, comprising the following steps of: with tripterygium ethyl acetate extract waste liquid subjected to the removal of triptolide and tripdiolide as a raw material, leaching by chloralkane; recrystallizing by using lower alcohol as a solvent; next, preparing the high-content sesquiterpenoids tripterygium alkaloid monomers by adopting inverse high-efficiency liquid phase semi-preparation chromatography; adopting on-line ultraviolet detection; collecting objectives; and obtaining four sesquiterpenoids tripterygium alkaloid monomers (wilfortrine, wilfordine, tripterygiumgyrine and wilforine) with content which is greater than 99.0 percent after freezing and drying. Due to the adoption of the disclosed preparation method, the separated product has the advantages of high purity, short process, low cost and easy industrialization.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of a high-content sesquiterpene tripterygium alkaloid monomer. Background technique [0002] Tripterygium wilfordii Hook.f. is a plant of the genus Tripterygium wilfordii Hook.f., whose roots, leaves, flowers and fruits are used as medicine for the treatment of autoimmune diseases, such as rheumatoid arthritis, chronic nephritis, lupus erythematosus, Contact dermatitis, etc. have a significant effect. According to the records of "Chinese Medicine Plants", tripterygine, tripterine, diterpene lactone, and dulcitol all have obvious anti-tumor activity, and have inhibitory effects on mouse leukemia and human nasopharyngeal carcinoma. The dilation of peripheral arterioles increases blood flow, reduces the resistance of peripheral blood flow, improves the obstruction of microcirculation, and has the effect of promoting blood circulation. It has hormo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/20
Inventor 蔡美强金米聪陈晓红
Owner ZHEJIANG GONGSHANG UNIVERSITY
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