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A kind of preparation method of high-purity diosmin

A diosmin, high-purity technology, applied in the field of separation and purification of high-purity drug diosmin, to achieve the effects of less environmental pollution, good selectivity, and good repeatability

Active Publication Date: 2020-08-07
杭州泽邦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the relevant technology for preparing high-purity diosmin has not been reported yet.

Method used

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  • A kind of preparation method of high-purity diosmin
  • A kind of preparation method of high-purity diosmin
  • A kind of preparation method of high-purity diosmin

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Experimental program
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Effect test

Embodiment 1

[0032] 1) Preparation of sample solution: Weigh 1.25 g of crude diosmin, add 50 mL of 0.2M NaOH solution, ultrasonically dissolve and filter for later use.

[0033] 2) Chromatographic separation process: the chromatographic filler UniPS TM Pack 10-300 in a 15mm*310mm chromatographic column, wash 200mL with deionized water, then inject the sample prepared in step 1) into the chromatographic column with a flow rate of 10mL / min, continue to use deionized water after loading Rinse until the first miscellaneous peak is gone, discard the eluent. After the baseline of the chromatographic column is stable, use the first eluent to elute until the main peak appears, and then use the second eluent to elute after the main peak has come out. Collect the eluent in 50mL per tube, and collect the eluent according to the time sequence of collection. Each tube was numbered, and the purity of diosmin was tested. The results are as follows:

[0034] Tube number 1 2 3 4 5 7 29 ...

Embodiment 2

[0038] 1) Preparation of sample solution: Weigh 60.0 g of crude diosmin, add 2.4 L of 0.2M NaOH solution, ultrasonically dissolve and filter for later use.

[0039] 2) Chromatographic separation process: the chromatographic filler UniPS TM Pack 10-300 in a 70mm*460mm chromatographic column, wash 4L with deionized water, then inject the sample prepared in step 1) into the chromatographic column with a flow rate of 50mL / min, continue to use deionized water after loading Rinse until the first miscellaneous peak is gone, discard the eluent. After the baseline is stable, use the first eluent to elute until the main peak appears, and then use the second eluent to elute after the main peak comes out. Use 2L of each eluent (numbers 3 to 6 are 1L, and the rest are 2L) ) collection, each tube is numbered according to the time sequence of collection, and the purity of diosmin is detected, the results are as follows:

[0040] Tube number 2 3 4 6 8 10 purity(%) 95.6...

Embodiment 3

[0044] 1) Preparation of sample solution: Weigh 60.0 g of crude diosmin, add 2.4 L of 0.2M NaOH solution, ultrasonically dissolve and filter for later use.

[0045] 2) Chromatographic separation process: the chromatographic filler UniPS TM Pack 10-300 in a 70mm*460mm chromatographic column, wash 4L with deionized water, then inject the sample prepared in step 1) into the chromatographic column with a flow rate of 50mL / min, continue to use deionized water after loading Rinse until the first miscellaneous peak is gone, discard the eluent. After the baseline is stable, use the first eluent to elute until the main peak appears, and then use the second eluent to elute after the main peak comes out. Use 2L of each eluent (numbers 3 to 6 are 1L, and the rest are 2L) ) collection, each tube is numbered according to the time sequence of collection, and the purity of diosmin is detected, the results are as follows:

[0046]

[0047] Then combine the diosmin eluents with a purity g...

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Abstract

The invention discloses a preparation method of high purity diosmin, which includes steps of: adding a diosmin crude product to an alkaline solvent to prepare a diosmin crude product solution; packinga polymer chromatographic packing into a chromatographic column, and loading the diosmin crude product solution on the chromatographic column through injection with a pump; with deionized water and an alkaline solvent being mobile phases, collecting a plurality of eluants and performing purity detection; mixing the high purity diosmin eluants, precipitating diosmin with acid, and filtering and washing the product, final product purity being higher than 99%. The method is economical and environment-friendly, is simple in operation, has good repeatability, is suitable for industrial preparationof high-purity diosmin, and has high economic and application benefits.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a method for separating and purifying high-purity drug diosmin. Background technique [0002] Diosmin (Diosmin), chemical name 7-{[6-oxo-(6-deoxy-α-L-mannose)-β-D-glucopyranose]oxyl}-5-hydroxyl-2-( 3-Hydroxy-4-methoxybenzene)-4H-L-benzopyran-4-one, soluble in dimethyl sulfoxide and strong alkaline solution, insoluble in water, methanol or ethanol, at 0.1mol / Very slightly soluble in L sodium hydroxide. Its structural formula is as follows: [0003] [0004] Diosmin was originally produced by the French company Servier and is a flavonoid intravenously active drug. Its main mechanism of action is to increase venous tone, improve microcirculation, and promote lymphatic return (Li Fengming, Tian Xiaodong, Hu Guowen, Chen Baoguo, Progress in Clinical Application of Diosmin, Modern Journal of Integrated Traditional Chinese and Western Medicine, 2012, 21(6)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/06
CPCC07H1/06C07H17/07
Inventor 潘远江黄德权方倩
Owner 杭州泽邦科技有限公司
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