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Method for preparing przewaquinone sodium sulfonate

A technology of sodium mesylate and purple salvia miltiorrhiza, applied in the field of medicine, can solve problems such as poor extraction, difficult extraction of purple salvia miltiorrhiza, high water solubility, etc.

Active Publication Date: 2014-06-18
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is that in order to overcome the defects of difficult extraction and low efficiency of salvia miltiorrhiza in the prior art, it provides sodium salvia miltiorrhiza sulfonate and its preparation method and application
The sodium sulfonate of salvia miltiorrhiza of the present invention has good water solubility, solves the problem that salvia salvia miltiorrhiza is too fat-soluble and poorly water-soluble to limit its application in the medical field, and has high purity, and the preparation method thereof has strong preparation ability and is easy to prepare. Large amount, short cycle, high efficiency, and reduce the use of organic solvents, continuous process operation is easy to carry out quality control and production

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  • Method for preparing przewaquinone sodium sulfonate
  • Method for preparing przewaquinone sodium sulfonate
  • Method for preparing przewaquinone sodium sulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Extraction of Tanshinone Compounds

[0065] Weigh 3 kg of crushed salvia miltiorrhiza (origin: Yunnan, Ganzi, Aba area), add 14 L of ethanol with a mass fraction of 90%, and extract in a 40°C water bath for 2 hours. Use 350-mesh filter cloth and filter paper to remove medicinal material residue and soil, concentrate the filtrate to 1.4L, let stand at 4°C for 24 hours, filter the filtrate after standing, and dry the obtained solid under vacuum at 40°C to obtain red tanshinone compound Solid powder 65.0g.

Embodiment 2

[0067] Sulfonation and post-treatment of tanshinone compounds

[0068] Take 60g of tanshinone compounds in Example 1, add 140mL of glacial acetic acid and 360mL of acetic anhydride, stir and cool the suspension to 0°C. While stirring, add 60mL of 98% concentrated sulfuric acid to 60mL of glacial acetic acid to prepare a mixed acid solution and let it stand to cool to room temperature. Add the mixed acid solution dropwise, maintain the reaction temperature at 10°C, and continue the heat preservation reaction for 90 minutes. Prepare dilution solution by 300mL petroleum ether + 600mL dichloromethane + 650mL purified water, stir and cool to 4°C. In the state of stirring, slowly add the above reaction liquid into the dilution liquid, and strengthen the cooling effect to ensure that the temperature of the system is lower than 25°C. Add 700g of sodium chloride to 2L of purified water, stir well to prepare saturated saline. The diluted reaction liquid was added into saturated brine...

Embodiment 3

[0070] Preparation and Purification of Sodium Violet Salvia Sulfonate

[0071] (1) Enrichment and purification: PrepStar SD-1 preparation system and L&L4002 chromatographic column (inner diameter 50mm) from Varian Company of the United States were used, and 160.0g of the company's PLRP-S reversed-phase C18 polymer filler (particle size 10μm, pore size 10nm) was self-packed. , The dynamic axial compression system is filled to a pressure of 650psi, and statically locked to a column bed height of 25cm. The enrichment conditions are: mobile phase A is 0.1% triethylamine-water, mobile phase B is 0.1% triethylamine-methanol, the flow rate is 100mL / min, the detection wavelength is 271nm, and the column temperature is room temperature. The mixture of tanshinone sulfonated liquid and mobile phase A with a volume ratio of 1:4 was loaded for 30 minutes, 80% mobile phase A+20% mobile phase B was equilibrated for 1 min, and the mobile phase A and mobile phase B were carried out according t...

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Abstract

The invention discloses a method for preparing przewaquinone sodium sulfonate. The preparation method comprises the following steps: separating tanshinone sulfonated liquid by adopting high performance liquid chromatography, wherein the conditions of the high performance liquid chromatography are as follows: the mobile phase A is 0.1% triethylamine-water, the mobile phase B is 0.1% triethylamine-methanol, or the mobile phase A is 0.1% diethylamine-water, the mobile phase B is 0.1% diethylamine-methanol, or the mobile phase A is 0.1% ethylamine-water, the mobile phase B is 0.1% ethylamine-methanol, or the mobile phase A is water, the mobile phase B is methanol, the percent is the volume percent of the component in the mobile phase, and the detection wavelength is 271nm. The preparation method disclosed by the invention is strong in preparation ability, large in preparation quantity, short in cycle, and high in efficiency, an organic solvent is reduced, the process operation continuity is strong, and mass control and production are easily carried out.

Description

technical field [0001] The invention relates to the field of medicaments, in particular to a preparation method of salvia miltiorrhiza sodium sulfonate. Background technique [0002] Salvia miltiorrhiza, also known as blood ginseng, red root, red root, blood root, is the rhizome of Labiatae (Salvia miltiorrhza), and its medicinal use was first recorded in "Shen Nong's Herbal Classic". Traditional Chinese medicine believes that its taste is bitter and slightly cold, and has the effects of promoting blood circulation and dysmenorrhea, dispelling blood stasis and relieving pain, clearing heart and eliminating troubles, cooling blood and eliminating carbuncle, and is suitable for treating irregular menstruation, dysmenorrhea, amenorrhea, metrorrhagia, leukorrhea, coronary heart disease, arterial Atherosclerosis, hyperlipidemia, angina pectoris, bruises and congestion, insomnia, neurasthenia, hepatitis B and other diseases are commonly used by patients with blood stasis and heat ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
Inventor 洪勇琚姝黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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