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Preparation method of hemostatic raw material dencichine

A technology of notoginseng and raw materials, applied in the field of preparation of hemostatic raw material notoginseng, can solve the problems of high cost, complicated reaction, environmental pollution and the like, and achieve the effects of short reaction time, simple operation and good environmental compatibility

Pending Publication Date: 2021-12-07
云南西草资源开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method of notoginsin as a raw material for hemostasis in view of the defects of high cost, complicated reaction, and easy environmental pollution in the existing synthesis method of notoginseng. To obtain an effective way to synthesize notoginseng, the process is simple, the cost is low, the operation is safe, the environment compatibility is good, and industrialized production can be implemented

Method used

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  • Preparation method of hemostatic raw material dencichine
  • Preparation method of hemostatic raw material dencichine
  • Preparation method of hemostatic raw material dencichine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 0.0125g of citric acid in 100mL of water, add 2mg of laccase (enzyme activity ≥0.5u / mg, provided by Shanghai Yuanye Biotechnology Co., Ltd.), slowly add 1mg of phenol and 100g of tryptophan while stirring, and react 2h, then add 100mL of 50% methanol containing 30g of monomethyl oxalate, pass in medical oxygen, keep the pressure at 5Mpa, and react for 8h. After the solution was allowed to stand still, solids were precipitated, washed with 50% acetone solution, and dried to obtain crude notoginsin, which was then dissolved in 100 mL of distilled water, and the pH value was adjusted to 2 with dilute hydrochloric acid to obtain a white precipitate, which was washed with 50% acetone solution , drying to obtain 15g notoginseng.

Embodiment 2

[0026] Dissolve 0.00625g of citric acid in 100mL of water, add 2mg of laccase (enzyme activity ≥0.5u / mg, provided by Shanghai Yuanye Biotechnology Co., Ltd.), slowly add 2mg of phenol and 120g of tryptophan while stirring, and react 4h, then add 80mL of 70% methanol containing 50g of monomethyl oxalate, feed medical oxygen, keep the pressure at 4Mpa, and react for 9h. After the solution was allowed to stand still, solids were precipitated, washed with 50% acetone solution, and dried to obtain crude notoginsin, which was then dissolved in 100 mL of distilled water, and the pH value was adjusted to 2 with dilute hydrochloric acid to obtain a white precipitate, which was washed with 50% acetone solution , drying to obtain 25g notoginseng.

Embodiment 3

[0028] Dissolve 0.01875g of citric acid in 100mL of water, add 2mg of laccase (enzyme activity ≥0.5u / mg, provided by Shanghai Yuanye Biotechnology Co., Ltd.), slowly add 3mg of phenol and 90g of tryptophan while stirring, and react 3h, then add 100mL of 80% methanol containing 40g of monomethyl oxalate, pass in medical oxygen, keep the pressure at 6Mpa, and react for 6h. After the solution was allowed to stand still, solids were precipitated, washed with 50% acetone solution, and dried to obtain crude notoginsin, which was then dissolved in 100 mL of distilled water, and the pH value was adjusted to 2 with dilute hydrochloric acid to obtain a white precipitate, which was washed with 50% acetone solution , drying to obtain 20g notoginseng.

[0029] Determination of the content of notoginseng

[0030] Chromatographic conditions: chromatographic column: Hypersil ODS2 (250 mm x4. 6 mm, 5 µm); mobile phase: methanol-water (70: 30); flow rate 1. 0 mL / min; detection wavelength: 214 ...

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Abstract

The invention belongs to the technical field of medical biology, and discloses a preparation method of a hemostatic raw material dencichine, which comprises the following steps of adding a laccase solution into a weakly acidic solution at normal temperature, adding tryptophan and phenol in a stirring state, reacting for 2-4 hours, adding a methanol solution containing oxalic acid monomethyl ester, reacting for 6-9 hours under the condition of a high-oxygen solution, after treatment, acquiring crude dencichine, and recrystallizing the crude dencichine to obtain pure dencichine. According to the method, tryptophan and phenol are adopted as reaction raw materials and react under the action of laccase to obtain diaminopropionic acid, diaminopropionic acid reacts with the methanol solution of oxalic acid monomethyl ester to obtain dencichine, the whole reaction process is easy to operate, dencichine with the purity of 80% or above can be obtained without using a strong base catalyst, meanwhile, the preparation method is mild in reaction condition and short in reaction time, the production efficiency is greatly improved, the production cost is saved, and industrial production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of medicine and biology, and relates to a preparation method of hemostatic raw material notoginseng. Background technique [0002] Panax notoginseng, also known as Tianqi, is a precious medicinal material in my country. It has the effects of dispelling blood stasis, stopping bleeding, reducing swelling and relieving pain. . The main monomeric hemostatic active substance contained in Panax notoginseng is notoginseng. Panax notoginseng, also known as astragalus, is a non-protein free amino acid in Panax notoginseng. It has hemostatic active ingredients. It can stop bleeding by increasing the number of platelets in the body and shorten the time of coagulation and bleeding. It is widely used in the treatment of traumatic bleeding etc., are the active ingredients of Yunnan Baiyao and many other traditional prescriptions. [0003] At present, there are many methods for the synthesis of notoginseng. Among them, R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/56C12P13/04
CPCC07C231/02C12P13/04C07B2200/07C07C233/56
Inventor 孙秋唐天鹏丁瑞赵平舟
Owner 云南西草资源开发有限公司
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