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Preparation method of salvianolic acid Y

A technology of salvianolic acid and salvianolic acid, applied in the field of medicine and chemical industry, can solve the problems of low purity, waste of resources, high cost, etc., and achieve the effect of high purity, few steps and simple operation

Pending Publication Date: 2019-07-09
TIANJIN TASLY ZHIJIAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] As a component of salvianolic acid extract, salvianolic acid Y has good medicinal activity and is an important component of salvia miltiorrhiza. Obtaining high-purity salvianolic acid Y can prepare standard substances and conduct new drug research, while the existing The method for obtaining salvianol Y in the technology is expensive, the purity is not high, and resources are wasted. For this reason, it is necessary to improve the efficiency

Method used

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  • Preparation method of salvianolic acid Y
  • Preparation method of salvianolic acid Y
  • Preparation method of salvianolic acid Y

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: A kind of preparation method of salvianolic acid Y

[0053] Step 1, enrichment of salvianolic acid Y

[0054] Take 500g of salvianolic acid extract, dissolve it in 1000ml of water (the weight-to-volume ratio of extract to water is 1:2), use a pH meter to detect the pH value is 5.5, load 100ml each time, add 3L MCI Gel glass In the chromatographic column (the ratio of extract mass to filler volume is 1:60), flow rate: 100ml / min. After sample loading, elute with 10% ethanol aqueous solution, flow rate: 100ml / min, take a sample every 300ml from the color of the bottom liquid, detect it by HPLC method, and compare it with the fingerprint of salvianolic acid extract, collect and combine Eluate containing salvianolic acid Y.

[0055] Adjust the pH value of the eluent to 3.0, add it again to a glass chromatographic column filled with 3LMCI Gel (the ratio of extract mass to filler volume is 1:6), wash 15L with water, discard the eluent, flow rate: 100ml / min. Th...

Embodiment 2

[0060] Embodiment 2: the enlarged preparation method of salvianolic acid Y

[0061] Step 1, enrichment of salvianolic acid Y

[0062] Take 1000g of salvianolic acid extract, dissolve it in 2000ml of water, use a pH meter to detect that the pH value is 5.5, load 100ml each time, add a 3L MCI Gel glass chromatographic column (the ratio of extract mass to filler volume is 1:60 ), flow rate: 100ml / min. After sample loading, elute with 10% ethanol aqueous solution, flow rate: 100ml / min, pick up a sample every 300ml from the color of the lower contact solution. Detected by HPLC method, and compared with the fingerprint of salvianolic acid extract at the same time, the eluate containing salvianolic acid Y in the 15th-25th bottle was combined.

[0063] Adjust the pH value of the eluent to 3.0, add it again to a 3L MCI Gel glass column (the ratio of extract mass to filler volume is 1:3), wash 15L with water, discard the eluent, flow rate: 100ml / min . Then elute with 95% ethanol, fl...

experiment example 1

[0068] Experimental example 1: Determination of the content of salvianolic acid Y

[0069] 1. Using high performance liquid chromatography, the specific conditions are as follows

[0070] Instruments: Agilent 1100 high performance liquid chromatography, quaternary pump, UV detector.

[0071] Chromatographic column: Agilent C18 analytical column (4.6mm×250mm, 5μm); mobile phase: gradient elution, see Table 1; flow rate: 1mL·min-1; detection wavelength: 280nm; column temperature: 30°C.

[0072] Table 1 Gradient of chromatographic conditions

[0073] Solvent time (min) 0 8 15 35 40 50 A: 80% acetonitrile + 20% B 10％ 22％ 26％ 39％ 10％ 10％ B: 0.02% phosphoric acid aqueous solution 90％ 78％ 74％ 61％ 90％ 90％

[0074] 2. Preparation of the sample solution to be tested: Take 10 mg of salvianolic acid Y, weigh it accurately, put it in a 25ml volumetric flask, dissolve it with methanol, and set the solution to the mark, and wait for the test.

[0...

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Abstract

The invention relates to a preparation method of salvianolic acid Y. The method comprises the following steps: step 1, salvianolic acid Y enrichment: taking a salvianolic acid extract, dissolving thesalvianolic acid extract with water, and adding the salvianolic acid extract solution into an MCI-GEL chromatographic column, conducting eluting with a 10%-20% ethanol aqueous solution, adjusting thepH value of the eluate, adding the treated eluate into an MCI-GEL chromatographic column, conducting eluting with 70-95% ethanol, recovering a solvent, and conducting concentrating to dryness to obtain a salvianolic acid Y enriched product; and step 2, fine separation: completely dissolving the salvianolic acid Y enriched product by a mobile phase with a mass-volume ratio of 2-3 times, conductingliquid phase separation by adopting dynamic axial pressurization, using an HPLC (High Performance Liquid Chromatography) method to detect and combine the eluates containing salvianolic acid Y, and conducting reduced-pressure concentration to obtain salvianolic acid Y single product, wherein the mobile phase adopts acetonitrile and a formic acid aqueous solution with a concentration of 0.01%.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a preparation method of salvianolic acid Y. Background technique [0002] Salvianolic acid Y (salvianolic acid Y), the chemical name is (2R,3S)-4-[(1E)-3-[(1R)-1-carboxy-2-(3,4-dihydroxyphenyl)ethyl Oxy]-3-oxo-1-propen-1-yl]-2-(3,4-dihydroxyphenyl)-2,3-dihydro-7-hydroxy-3-benzofurylcarboxylic acid-[ (1R)-1-carboxy-2-(3,4-dihydroxyphenyl)] ethyl ester is an epimer of salvianolic acid B isolated from salvianolic acid extract, and has relatively Strong free radical scavenging effect, its structure is shown in formula Ⅰ: [0003] [0004] CN105218495A (the application number is 201410226328.5) discloses salvianolic acid Y and its preparation method. The preparation method is as follows: decocting the salvia miltiorrhiza medicinal material for 3 times, adding 3-6 times the amount of water each time, decocting for 0.5-2 hours, Combine the decoctions, cool to 8-14°C, ...

Claims

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Application Information

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IPC IPC(8): C07D307/86
CPCC07D307/86
Inventor 罗学军阎红田介峰李淑明宋兆晖何毅李伟岳洪水周水平鞠爱春
Owner TIANJIN TASLY ZHIJIAO PHARMA
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