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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AI-Extracted 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 puri...

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Method used

[0026] The ultrafiltration of the extract is used to remove macromolecular substances, so as to avoid serious emulsification in the subsequent extraction pro...

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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.

Application Domain

Carboxylic compound separation/purification

Technology Topic

Macromolecular SubstancesUltrafiltration +3

Examples

Experimental program(2)

Example Embodiment

[0031] Example 1

[0032] 1. Crushing and degreasing

[0033] 2 kg of salvia root → crushed (1~3mm) → degreasing with petroleum ether (4L×3) → drying → defatted salvia miltiorrhiza powder.

[0034] 2: Extraction, ultrafiltration, concentration

[0035] Defatted salvia powder→16L deionized water extraction (80℃, 2 hours)→12L deionized water extraction (80℃, 2 hours)→8L deionized water extraction (80℃, 2 hours)→combination→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 under nitrogen protection for 2 hours → add 2 mol.L -1 HCl to adjust the pH to 3.0.

[0038] 4: Extraction

[0039] Acidified Danshen transformation solution → ethyl acetate extraction (600 mL×5) → ethyl acetate recovery under reduced pressure → crude Danshensu (18 g, light yellow powder, Danshensu purity 65%, protocatechuic aldehyde 16%).

[0040] 5: Silica gel chromatography

[0041] Crude Danshensu (18g)→add diatomaceous earth (45g) and mix well→vacuum drying→solid powder→put on stainless steel column (silica gel 400g, φ50×500)→step elution (ethyl acetate 3L, ether/acetic acid) Ethyl ester/methanol mixture (6:20:4) 6L, methanol 3L; flow rate 10~20mL/min) → collection in sections (100~150mL per section) → merge in sections (after TLC and HPL detection, press Salvia miltiorrhiza The two parts of Su and protocatechualdehyde were combined) → part of Danshensu → vacuum concentration to recover solvent → Danshensu (11.5g).

Example Embodiment

[0042] Example 2

[0043] 1: Extraction, ultrafiltration, concentration

[0044] Salvia Root 100kg→Pulverization (1~3mm)→800L Deionized Water Extraction (80℃, 2 Hours)→600L Deionized Water Extraction (80℃, 2 Hours)→400L Deionized Water Extraction (80℃, 2 Hours) →Merge →Ultrafiltration →Concentrate under reduced pressure to 100L.

[0045] 2: Conversion

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

[0047] 3: Extraction

[0048] Acidified Danshen transformation solution→ethyl acetate extraction (30L×5)→recovery of ethyl acetate under reduced pressure→crude Danshensu (920 g, light yellow powder, Danshensu purity 67%, protocatechuic aldehyde 14%).

[0049] 4: Silica gel chromatography

[0050] Crude Danshensu (920g)→adding diatomite (2.5kg) and mixing→vacuum drying→solid powder→put on stainless steel column (silica gel 20kg, φ200×1500)→step elution (ethyl acetate 150L, ether/ Ethyl acetate/methanol mixed solution (6:20:4) 300L, methanol 150L; flow rate 400-450mL/min) → segmented collection (4-5L per segment) → segmented merge (after TLC and HPL detection, press The two parts of Danshensu and protocatechuic aldehyde were combined)→Part of Danshensu→vacuum concentration to recover solvent→Danshensu (487g).

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Reduce solvent loss
Improve extraction rate

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Improve processing power High recovery rate Low cost Chemistry Alcohol

Process for preparing Danshensu

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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