Method for rapidly preparing tripterine chemical reference substance from Common Threewingnut Root extract

A technology of tripterygenin chemistry and tripterygenin, which is applied in the field of rapid preparation of tripterygenin chemical reference substances from tripterygium wilfordii extract, can solve the problems of small preparation flux and unguaranteed purity, and achieve rapid Effects of recycling, improving purity, and reducing costs

Inactive Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the existing methods, those prepared by recrystallization use a large amount of halogenated hydrocarbons, and the purity cannot be guaranteed, while the reversed-pha

Method used

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  • Method for rapidly preparing tripterine chemical reference substance from Common Threewingnut Root extract
  • Method for rapidly preparing tripterine chemical reference substance from Common Threewingnut Root extract
  • Method for rapidly preparing tripterine chemical reference substance from Common Threewingnut Root extract

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Embodiment 1

[0029] 1) Ethyl acetate extraction

[0030] 500g of the root of Tripterygium wilfordii, extracted 3 times with 1500mL of absolute ethanol, 3 hours each time, combined the three extracts, recovered under reduced pressure to obtain about 31g of the total extract, dispersed with about 120mL of water, and extracted 3 times with ethyl acetate , about 150mL each time. The extracts were combined and recovered under reduced pressure to obtain about 15 g of ethyl acetate.

[0031] 2) Separation by silica gel column chromatography

[0032] Add about 15g of silica gel to mix well, dry under reduced pressure, and separate by silica gel vacuum chromatography (40cm*5cm), use 5 times column volume of petroleum ether: ethyl acetate (volume ratio 4:1) ), petroleum ether: ethyl acetate (volume ratio 2:1), petroleum ether: ethyl acetate (volume ratio 1:1) step gradient elution, thin-layer chromatography detection, with petroleum ether: ethyl acetate (volume ratio 2 : 1) as developer, GF254 fl...

Embodiment 2

[0038] 1) Ethyl acetate extraction

[0039] 1000g of tripterygium twig root, extracted once with 3000mL of 80% ethanol / water for 3 hours, recovered under reduced pressure to obtain about 52g of total extract, dispersed with about 250mL of water, and extracted once with ethyl acetate, about Use 300mL. Recover under reduced pressure to obtain about 26 g of ethyl acetate.

[0040] 2) Separation by silica gel column chromatography

[0041] Add about 26g of silica gel to mix well, dry under reduced pressure, and separate by silica gel decompression chromatography (45cm*6cm), and use 5 times the column volume of petroleum ether: ethyl acetate (volume ratio 4:1) ), petroleum ether: ethyl acetate (volume ratio 2:1), petroleum ether: ethyl acetate (volume ratio 1:1) step gradient elution, thin-layer chromatography detection, with petroleum ether: ethyl acetate (volume ratio 2 : 1) as developer, GF254 fluorescent plate, dark spots were inspected at 254nm of ultraviolet lamp, the elua...

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Abstract

The invention relates to a new method for rapidly preparing a highly pure tripterine chemical reference substance from Common Threewingnut Root. The tripterine chemical reference substance with the purity of above 98% can be obtained through ethanol extraction of a Common Threewingnut Root medicinal material, ethyl acetate extraction, silica gel column chromatography, high performance chromatographic separation and gel purification. The method has the advantages of simple steps, easy large-scale production and high purity.

Description

technical field [0001] The invention relates to a new preparation process for rapidly preparing a chemical reference substance of tripterygium wilfordii from tripterygium wilfordii. It mainly includes extraction and extraction, silica gel column separation, rapid high performance liquid phase preparation and gel purification. The structural formula of tripterine is as follows: [0002] Background technique [0003] In traditional medicine, Tripterygium wilfordii is a commonly used medicinal plant of the genus Tripterygium, which is often used to treat rheumatoid arthritis, itchy skin, girdle sores and leprosy reactions. Modern pharmacological experiments have shown that Tripterygium wilfordii has anti-inflammatory, anti-oxidant, immunosuppressive, anti-fertility, antibacterial, analgesic, anti-tumor effects. Tripterine, also known as celastrol, is a red needle-like crystal, a carbon pentacyclic triterpene, widely distributed in the medicinal plants of the genus Triptery...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 肖红斌洪志来高明哲卓荣杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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