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Preparation method of high-purity troxerutin

A high-purity, rutin technology, applied in the field of preparation of high-purity troxerutin, can solve problems such as product loss, low troxerutin yield, etc., and achieve the effect of improving yield and purity

Active Publication Date: 2015-03-25
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the production process of troxerutin, the impurities produced include unreacted rutin, monohydroxyethyl rutin, dihydroxyethyl rutin, tetrahydroxyethyl rutin and some compounds without ultraviolet absorption. Pharmacopoeia quality standard, using traditional technology, multiple recrystallization of methanol will cause a lot of product loss, especially the yield of troxerutin for injection is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Mix rutin (100g) and sodium methoxide (8g) evenly and put them into an autoclave, pour ethylene oxide (32g) into 300ml of methanol, then pour into the autoclave, close the autoclave, and The temperature is up to 70°C. At this time, the pressure in the high-pressure reactor is about 0.3 MPa. After 4 hours of reaction, sampling and monitoring are started. HPLC detects that the content of trihydroxyethyl rutin is the highest. Stop the reaction, and adjust the pH of the reaction solution to 5 with dilute hydrochloric acid. -6. The filtrate is evenly divided into two parts, one part is stirred, cooled and crystallized, and then suction-filtered to obtain troxerutin with relatively high purity, and the other part is obtained by rotating methanol to obtain troxerutin with relatively high weight.

Embodiment 2

[0016] Put rutin (150g) and sodium methoxide (10g) into the autoclave after mixing evenly, pour ethylene oxide (50g) into 450ml of methanol, then pour it into the autoclave, close the autoclave, and The temperature is up to 80°C. At this time, the pressure in the high-pressure reactor is 0.5 MPa. After 4 hours of reaction, start sampling and monitoring. HPLC detects that the content of trihydroxyethyl rutin is the highest. Stop the reaction, and adjust the pH of the reaction solution to 5-6 with dilute hydrochloric acid. . The filtrate is evenly divided into two parts, one part is stirred and cooled to crystallize, and then suction-filtered to obtain troxerutin with relatively high purity, and the other part is obtained by spinning out methanol to obtain troxerutin with relatively high weight.

Embodiment 3

[0018] Mix rutin (100g) and sodium ethoxide (10g) evenly and put them into an autoclave, pour ethylene oxide (25g) into 500ml of methanol, then pour into the autoclave, close the autoclave, and High temperature to 50°C. At this time, the pressure in the high-pressure reactor is about 0.2 MPa. After 4 hours of reaction, start sampling and monitoring. HPLC detects that the content of trihydroxyethyl rutin is the highest. Stop the reaction, and adjust the pH of the reaction solution to 5- 6. The filtrate is evenly divided into two parts, one part is stirred and cooled to crystallize, and then suction-filtered to obtain troxerutin with relatively high purity, and the other part is obtained by spinning out methanol to obtain troxerutin with relatively high weight.

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Abstract

The invention discloses a preparation method of high-purity troxerutin. According to the preparation method of the high-purity troxerutin, the synthesis and refining processes of the troxerutin are improved; sodium methoxide or sodium ethoxide is selected as a catalyst, supercritical CO2 is selected for extraction and crystallization refining of the troxerutin, and finally, the troxerutin of which the yield and the purity both are greatly improved in contrast with a traditional process can be obtained.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of high-purity troxerutin. Background technique [0002] Troxerutin has anticoagulant and antithrombotic effects, and is suitable for hemiplegia, aphasia, arteriosclerosis, thrombophlebitis, varicose veins, chronic venous insufficiency, central retinitis, diabetic Treatment of retinitis and edema caused by increased vascular permeability. The traditional production method of troxerutin is to use natural rutin and ethylene oxide as raw materials, strong base as catalyst, water as solvent, and through hydroxyethylation to obtain hydroxyethyl rutin mainly composed of trihydroxyethylrutin. A mixture of rutin. However, using a strong base as a catalyst and water as a solvent may easily cause side reactions such as hydrolysis and oxidation in the later stage of the reaction, which increases the difficulty of purification of trihydroxyethyl...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/00C07H1/06
CPCY02P20/54
Inventor 谭绪霞李世宁姜玉钦毛龙飞齐庆华董文佩张玮玮徐桂清李伟
Owner HENAN NORMAL UNIV
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