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Method for detecting salvianolic acid A related substances

A related substance, salvianolic acid technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of poor separation of salvianolic acid A and poor method specificity.

Inactive Publication Date: 2021-05-18
JIANGZI QINGFENG PHARMACEUTICALS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there are many patents and open documents about the method for the determination of salvianolic acid A content. The mobile phase used in the method of high performance liquid chromatography determination has acetonitrile, formic acid, acetonitrile-water, formic acid-water, etc. Or its combination, but the technical scheme disclosed in the prior art has poor separation of each related substance of salvianolic acid A, and the specificity of the method is not strong

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  • Method for detecting salvianolic acid A related substances
  • Method for detecting salvianolic acid A related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: the preparation of salvianolic acid A test sample

[0022] Take the Danshen medicinal material, crush it into particles with a diameter of about 2mm, add 9 times the amount each time, soak in water at 85°C for 3 times, and stir at a speed of 20 rpm, and extract with warm soaking for 2.5 hours each time; the extract is concentrated under reduced pressure to relative density 1.25 (60°C), add ethanol to make the alcohol content 70%, let it stand, filter, and recover the ethanol from the filtrate under reduced pressure and concentrate until there is no alcohol smell; add water to dilute to 10mg of salvianolic acid B per 1ml, and use 20% lemon in the aqueous solution Adjust the pH to 3.5 with sodium phosphate, add 0.4% PdCl3 as a catalyst, heat and convert at 132°C for 3.5 hours, adjust the pH of the conversion liquid to 2.6 with 20% acetic acid, centrifuge, and concentrate the supernatant under reduced pressure to contain salvianolic acid per 1ml A5 mg was sep...

Embodiment 2

[0023] Embodiment 2: High performance liquid chromatography detects the content of related substances of salvianolic acid A

[0024] 1. Solution preparation

[0025] Diluent solution: 30% acetonitrile (containing 0.1% phosphoric acid) in water as a diluent.

[0026] Reference substance solution: Accurately measure 10mg of salvianolic acid A working reference substance, put it in a 100ml measuring bottle, add diluent to dissolve and dilute to the mark, then accurately measure 0.7ml, put it in a 100ml measuring bottle, add diluent to dilute to the mark as a control solution.

[0027] Need testing solution: Accurately measure 10 mg of salvianolic acid A, place it in a 50 ml measuring bottle, add diluent to dissolve and dilute to a solution containing 0.2 mg of salvianolic acid A per 1 ml, shake well, and use it as the testing solution.

[0028] 2. Chromatographic conditions

[0029] High performance liquid chromatograph model: Agilent1260.

[0030] Chromatographic column: ACE...

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Abstract

The invention relates to a method for detecting related substances of salvianolic acid A by using a high performance liquid chromatography, which optimizes and selects a mobile phase, detects the related substances by using a gradient elution method, has better sensitivity and separation degree compared with the prior art, and is beneficial to quality control and safe application of a salvianolic acid A product.

Description

technical field [0001] The invention relates to the field of drug detection and analysis, in particular to a method for determining salvianolic acid A related substances by high performance liquid chromatography. Background technique [0002] Salvianolic acid A (Salvianic acid A) is transformed from salvianolic acid B in the labiatae plant Salvia miltiorrhiza. High-purity salvianolic acid A was obtained after purification by macroporous resin and normal phase silica gel. Salvianolic acid A is light yellow powder, easily soluble in water, ethanol, methanol, acetonitrile, tert-butyl methyl ether, N,N-dimethylformamide, dimethyl sulfoxide; almost insoluble in cyclohexane, It is unstable to light and heat, and its structural formula is as follows: [0003] [0004] In the process of preparing medicines, the separation technology of impurities and active ingredients is particularly important to ensure the quality of medicines. The structure, physical and chemical properties...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/32G01N30/34G01N30/54G01N30/60
CPCG01N30/02G01N30/32G01N30/34G01N30/54G01N30/60G01N2030/324
Inventor 刘艳红邓双炳黄冰峰张毅余水平周舟刘芳芳周鹏钟仁清
Owner JIANGZI QINGFENG PHARMACEUTICALS INC