Method for reducing organic solvent residue in tripterygium glycoside

A technology of tripterygium wilfordii polyglycoside and organic solvent, which is applied in the field of refining tripterygium wilfordii polyglycosides to achieve the effects of stable quality and reducing organic solvent residues

Active Publication Date: 2014-03-05
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

[0024] Take the semi-finished product of tripterygium wilfordii polyglycoside (the product obtained after chromatography in the production process of tripterygium wilfordii polyglycoside, the same below) 10Kg, add 1.5 times (15L) of absolute ethanol, fully stir to make the dissolution uniform. Concentrate the ethanol solution to recover most of the ethanol and drain under reduced pressure to obtain a dry powder. After passing through a 40-mesh sieve, the weight is 9.82Kg; another 50Kg of purified water is placed in an open pot and the steam is heated to 60℃ ( Thermometer detection), put this hot water in a stainless steel tank, add 9.82Kg of powder while stirring, stir for 15 minutes after it is added completely, and let it stand overnight. On the second day, the upper layer of clear water was siphoned out, and the lower layer of water-containing sediment was centrifuged to dry with a three-foot centrifuge. The wet product of Tripterygium wilfordii was weighed 27.14Kg. Put this...

Embodiment 2

[0027] Take 30Kg of the semi-finished product of Tripterygium wilfordii polyglycosides, add 3 times (90L) of absolute ethanol, stir thoroughly to make the dissolution uniform. Then concentrate the ethanol solution to recover most of the ethanol, and then drain under reduced pressure to obtain a dry powder, which is weighed 28.42Kg after passing through a 40-mesh sieve; another 100Kg of purified water is placed in an open pot and heated to 62℃ ( Thermometer detection), put this hot water in a stainless steel storage tank, add 28.42Kg of powder while stirring, stir for 30 minutes after it is completely added, and let it stand overnight. On the second day, the upper layer of clear water was siphoned out, and the lower layer of water-containing sediment was centrifuged to dry with a three-foot centrifuge. This wet product of Tripterygium wilfordii weighs 73.22Kg. Put this 73.22Kg of Tripterygium wilfordii wet product in a ZG-15 vacuum drying oven, turn on the steam to make the temp...

Embodiment 3

[0030] Take 100Kg of the semi-finished product of Tripterygium wilfordii polyglycosides, add 1.5 times (150L) of absolute ethanol, stir well to make the dissolution uniform. Concentrate this ethanol solution to recover most of the ethanol and drain under reduced pressure to obtain a dry powder. After passing through a 40-mesh sieve, the weight is 98.72Kg; another 300Kg of purified water is placed in an open pot and heated to 65°C with steam ( Thermometer detection), put this hot water in a stainless steel tank, add 98.72Kg of powder while stirring, stir for 30 minutes after it is completely added, and let it stand overnight. On the second day, the upper layer of clear water was siphoned out, and the lower layer of water-containing sediment was centrifuged to dry with a three-foot centrifuge. The wet product of Tripterygium wilfordii weighs 289.14Kg. Put this wet product of Tripterygium wilfordii 289.14Kg in four ZG-15 vacuum drying ovens, turn on the steam to make the temperatu...

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PUM

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Abstract

The invention relates to a method for reducing an organic solvent residue in tripterygium glycoside. Organic solvents (mainly comprising ethanol and chloroform) are adopted to carry out collection, extraction, chromatography and the like in a production technology of the tripterygium glycoside, and the problem of an unstable index of the organic solvent residue in the tripterygium glycoside is generated at present. The method comprises the following steps: dissolving a tripterygium glycoside semi-finished product by absolute ethyl alcohol, and fully agitating to evenly dissolve; concentrating the obtained tripterygium glycoside ethanol solution, and pumping out at reduced pressure after recovering ethanol, so as to obtain a powdery dry product; and obtaining the tripterygium glycoside product by adopting a method of combining warm water precipitation with low-temperature vacuum drying. By adopting the method, the organic solvent residue in the tripterygium glycoside can be effectively reduced, and the quality is stable.

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 ...

Claims

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Application Information

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Patent Type & Authority Applications(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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