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Process for preparing Danshensu

A technology of danshensu and salvia miltiorrhiza, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of conflicting purity, yield and processing capacity, low processing capacity, high cost, etc., and achieve low cost and high recovery rate High, guaranteed separation performance

Inactive Publication Date: 2005-09-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adsorption resin and ion exchange resin method product quality is better (purity is more than 80%), but yield is only about 30%
Because the properties of water-soluble impurities are similar to those of Danshensu, and the amount is large, the purification of Danshen injection by silica gel chromatography has low yield, low processing capacity and high cost
In a word, none of the above-mentioned methods solves the three contradictory problems of purity, yield and throughput at the same time.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Crushing and degreasing

[0033] Salvia root 2 kg → crush (1 ~ 3mm) → petroleum ether defatted (4L × 3) → dry → defatted Salvia powder.

[0034] 2: Extraction, ultrafiltration, concentration

[0035] Defatted salvia miltiorrhiza powder → 16L deionized water extraction (80°C, 2 hours) → 12L deionized water extraction (80°C, 2 hours) → 8L deionized water extraction (80°C, 2 hours) → merge → ultrafiltration → decompression Concentrate to 2L.

[0036] 3: Conversion

[0037] Salvia miltiorrhiza concentrate → add sodium bisulfite (10g) and saturated NaOH to adjust to pH 9~10 → stir for 2 hours under nitrogen protection → add 2mol.L -1 Adjust the pH to 3.0 with HCl.

[0038] 4: Extraction

[0039] Acidified Danshen conversion liquid→ethyl acetate extraction (600mL×5)→recovering ethyl acetate under reduced pressure→danshensu crude product (18g, light yellow powder, danshensu purity 65%, protocatechualdehyde 16%).

[0040] 5: Silica gel chromatography

[0041] Danshens...

Embodiment 2

[0043] 1: Extraction, ultrafiltration, concentration

[0044] Salvia miltiorrhiza root 100kg→crushed (1~3mm)→800L deionized water extraction (80℃, 2 hours)→600L deionized water extraction (80℃, 2 hours)→400L deionized water extraction (80℃, 2 hours) → Combine → Ultrafiltration → Concentrate under reduced pressure to 100L.

[0045] 2: Conversion

[0046] Salvia miltiorrhiza concentrate → add sodium bisulfite (500g) and saturated NaOH to adjust the pH to 9~10 → stir for 2 hours under nitrogen protection → add 2mol.L -1 Adjust the pH to 3.0 with HCl.

[0047] 3: Extraction

[0048] Acidified Danshen transformation solution→ethyl acetate extraction (30L×5)→recovering ethyl acetate under reduced pressure→danshensu crude product (920g, light yellow powder, danshensu purity 67%, protocatechualdehyde 14%).

[0049] 4: Silica gel chromatography

[0050] Danshensu crude product (920g) → add diatomaceous earth (2.5kg) and mix well → vacuum dry → solid powder → put on a stainless steel...

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PUM

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Abstract

The invention relates to a method for preparing danshensu which comprises: getting extract liquid from the water or alcohol with danshensu and danshensu precursors using danshen as the materials, inverting the danshensu precursors of the said extract liquid into danshensu using diluted alkali, super filtering the macromolecular substance of the said extract liquid after conversion using a hyperfiltration membrane, extracting the danshensu from the said extract liquid after hyperfiltration, and separating the said extraction using the normal phase chromatography to get the danshensu.

Description

Technical field: [0001] The invention relates to a preparation method of medicinal danshensu, especially a preparation method whose process sequence is extraction→dilute alkali conversion→ultrafiltration→extraction→normal phase chromatography. Background technique: [0002] Salvia miltiorrhiza has the effects of expanding arteries, increasing coronary artery flow, improving myocardial anti-hypoxia ability, inhibiting platelet aggregation, anticoagulation, improving blood circulation, anti-oxidation, inhibiting endogenous cholesterol synthesis, anti-atherosclerosis and enhancing learning and memory. It is widely used in the prevention and treatment of diseases such as coronary heart disease, stroke, hyperlipidemia and peptic ulcer. Studies have shown that the water-soluble component Danshensu is its main active ingredient, and the clinical preparation is an injection with Danshensu as the main component. [0003] At present, Danshen injection is a brown clear liquid. In clin...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C59/52
Inventor 杨凌何克江杨义
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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