A kind of method for reducing organic solvent residue in tripterygium glycosides

A technology of tripterygium glycosides and organic solvents, applied in the field of refining tripterygium glycosides, can solve problems such as unstable organic solvent residue indicators, achieve the effect of reducing organic solvent residues and stabilizing quality

Active Publication Date: 2015-12-30
浙江得恩德制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the unstable problem of the organic solvent residual index in the existing tripterygium glycosides, and to provide a Method for residual organic solvents to ensure consistent quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 10Kg of the semi-finished product of tripterygium glycosides (the product obtained after chromatography in the production process of tripterygium glycosides, the same below), add 1.5 times (15 L) of absolute ethanol, stir well to dissolve evenly. Concentrate the ethanol solution, recover most of the ethanol, and dry it under reduced pressure to obtain a dry product powder, which is weighed as 9.82Kg after passing through a 40-mesh sieve; another 50Kg of purified water is placed in an open pot and heated to 60°C ( Thermometer detection), put the hot water into a stainless steel storage tank, add 9.82Kg powder while stirring, stir for 15 minutes after adding completely, and let it stand overnight. The next day, siphon out the clear water in the upper layer, and dry the water-containing sediment in the lower layer with a three-legged centrifuge. The wet product of Tripterygium wilfordii weighs 27.14Kg. Put 27.14Kg of the wet product of Tripterygium wilfordii in a ZG-1...

Embodiment 2

[0024] Take 30Kg of the semi-finished product of tripterygium glycosides, add 3 times (90L) of absolute ethanol, stir well to dissolve evenly. Concentrate the ethanol solution, recover most of the ethanol, and dry it under reduced pressure to obtain a dry product powder, which is weighed as 28.42Kg after passing through a 40-mesh sieve; another 100Kg of purified water is placed in an open pot and heated to 62°C ( Thermometer detection), put the hot water into a stainless steel storage tank, add 28.42Kg powder while stirring, stir for 30 minutes after adding completely, and let it stand overnight. The next day, siphon out the clear water in the upper layer, and dry the water-containing sediment in the lower layer with a three-legged centrifuge. The wet product of Tripterygium wilfordii weighs 73.22Kg. Put 73.22Kg of the wet product of Tripterygium wilfordii in a ZG-15 vacuum drying oven, turn on the steam to keep the temperature at about 55°C, and turn on the vacuum pump to kee...

Embodiment 3

[0027] Take 100Kg of semi-finished tripterygium glycosides, add 1.5 times (150L) of absolute ethanol, stir well to dissolve evenly. Concentrate the ethanol solution, recover most of the ethanol, and dry it under reduced pressure to obtain a dry product powder, which is weighed as 98.72Kg after passing through a 40-mesh sieve; another 300Kg of purified water is placed in an open pot and heated to 65°C ( Thermometer detection), put the hot water into a stainless steel storage tank, add 98.72Kg powder while stirring, stir for 30 minutes after adding completely, and let it stand overnight. The next day, siphon out the clear water in the upper layer, and dry the water-containing sediment in the lower layer with a three-legged centrifuge. The wet product of Tripterygium wilfordii weighs 289.14Kg. Put 289.14Kg of the wet product of Tripterygium wilfordii in four ZG-15 vacuum drying ovens, turn on the steam to keep the temperature at about 55°C, and turn on the vacuum pump to keep the...

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PUM

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Abstract

The invention relates to a method for reducing residual organic solvents in tripterygium glycosides. In the production process of tripterygium glycosides, organic solvents (mainly ethanol and chloroform) must be used for extraction, extraction, chromatography, etc. Currently, there is a problem of unstable residual indicators of organic solvents in tripterygium glycosides. The present invention dissolves the semi-finished tripterygium glycosides with absolute ethanol, and fully stirs to make the dissolution uniform; concentrates the obtained tripterygium glycosides ethanol liquid, recovers the ethanol, and decompresses and drains to obtain a powdery dry product; then uses warm water to precipitate Combined with the low-temperature vacuum drying method, the tripterygium glycosides finished product is obtained. The invention can effectively reduce the residual organic solvent in the tripterygium glycosides, and has stable quality.

Description

technical field [0001] The invention relates to a method for refining tripterygium glycosides, in particular to a method for reducing residual organic solvents in tripterygium glycosides. Background technique [0002] Tripterygium wilfordii is the extract of the peeled root of Tripterygium wilfordii, which has anti-inflammatory and inhibitory effects on cellular immunity and humoral immunity, and is used for the treatment of rheumatoid arthritis, nephrotic syndrome, and autoimmune hepatitis. [0003] In recent years, studies have found that Tripterygium wilfordii preparations have significant clinical effects on organ transplant rejection, autoimmune diseases, nephrotic syndrome, and cancer. Antibacterial, analgesic, anti-leukemia treatment and other pharmacological effects. [0004] The crude product of Tripterygium wilfordii polyglycosides obtained through extraction, concentration, extraction, and chromatography contains a large amount of substances harmful to human body...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/37
Inventor 吕文辉刘法千鲍立曾
Owner 浙江得恩德制药股份有限公司
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