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Method for separating and detecting mercaptoacetic acid

A technology of thioglycolic acid and aqueous solution, which is applied in the field of analytical chemistry and can solve problems such as the influence of the accuracy of test results, high toxicity of thioglycolic acid, and instability of thioglycolic acid.

Pending Publication Date: 2022-06-07
SUNSHINE LAKE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The chemical formula of thioglycolic acid is C 2 h 4 o 2 S, the structural formula is HSCH 2 COOH, which is often used as an intermediate material for the synthesis of raw materials, is also used as an antioxidant and stabilizer in pharmaceutical preparations to enhance the stability of the main drug and extend the validity period of pharmaceutical preparations. However, thioglycolic acid has high toxicity, so it needs control it
[0003] At present, the commonly used detection method for thioglycolic acid is high performance liquid chromatography, and it is also reported that ion chromatography, thin layer chromatography, etc. are used for detection. Acetic acid is oxidized or complexed by heavy metals and becomes unstable at lower concentrations, thus affecting the accuracy of the test results
In order to avoid the instability of thioglycolic acid during detection, and to better and more accurately control product quality and ensure drug safety, it is necessary to study the analysis and detection method suitable for thioglycolic acid in drugs

Method used

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  • Method for separating and detecting mercaptoacetic acid
  • Method for separating and detecting mercaptoacetic acid
  • Method for separating and detecting mercaptoacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Instruments and Conditions

[0068] Column: Waters HSS T3 column, 4.6*100mm, 2.5μm;

[0069] Detector: MS (triple quadrupole); Scanning mode: MRM (parent ion m / z=181, product ion m / z=91, collision voltage 20V, collision energy 2V, negative electrode);

[0070] Flow rate: 1.0mL / min; Column temperature: 30℃; Injection volume: 20μL;

[0071] Mobile phase A: 0.1% formic acid in water (V:V); mobile phase B: acetonitrile;

[0072] Elution ratio:

[0073] 0-3min: mobile phase A: mobile phase B (V / V)=95:5;

[0074] 3.1-10min: mobile phase A: mobile phase B (V / V)=10:90;

[0075] Running time: 15min; post-run: 5min.

[0076] Experimental procedure

[0077] Diluent: ultrapure water;

[0078] Ammonia solution: Pipette 0.5mL of 25% ammonia into 500mL of ultrapure water and shake well;

[0079] Hydrogen peroxide solution: Pipette 3.5mL of 30% hydrogen peroxide solution into 100mL of ultrapure water and shake well;

[0080] Blank solution: pipette 1.0 mL of ammonia solution...

Embodiment 2

[0105] Instruments and Conditions

[0106] Column: Waters HSS T3 column, 4.6*100mm, 2.5μm;

[0107] Detector: MS (triple quadrupole); Scanning mode: MRM (parent ion m / z=181, product ion m / z=91, collision voltage 20V, collision energy 2V negative electrode);

[0108] Flow rate: 1.0mL / min; Column temperature: 30℃; Injection volume: 20μL;

[0109] Mobile phase A: 0.1% formic acid in water (V:V); mobile phase B: acetonitrile;

[0110] Elution ratio:

[0111] 0-3min: mobile phase A: mobile phase B (V / V)=95:5;

[0112] 3.1-10min: mobile phase A: mobile phase B (V / V)=10:90;

[0113] Running time: 15min; post-run: 5min.

[0114] Experimental procedure

[0115] Diluent: ultrapure water;

[0116] Ammonia solution: Pipette 0.5mL of 25% ammonia water to 500mL of ultrapure water and shake well;

[0117] Hydrogen peroxide solution: Pipette 3.5mL of 30% hydrogen peroxide solution into 100mL of ultrapure water and shake well;

[0118] Blank solution: pipette 1.0 mL of ammonia solut...

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Abstract

The invention relates to a method for separating and detecting mercaptoacetic acid, and belongs to the field of analytical chemistry. According to the method, an aqueous solution of hydrogen peroxide and mercaptoacetic acid are subjected to an oxidation reaction under an alkali adding condition, and an oxidation product is detected by HPLC-MS; during detection, a chromatographic column taking high-strength silica gel particles as a filler is adopted, a mobile phase is divided into a phase A and a phase B, the phase A is an aqueous solution of acid, and the phase B is acetonitrile. The method is high in sensitivity, good in specificity and reliable in accuracy.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and detecting thioglycolic acid. Background technique [0002] The chemical formula for thioglycolic acid is C 2 H 4 O 2 S, the structural formula is HSCH 2 COOH, which is often used as an intermediate material in the synthesis of raw materials, is also used as an antioxidant and stabilizer in pharmaceutical preparations to enhance the stability of the main drug and prolong the validity period of the pharmaceutical preparation, but thioglycolic acid has high toxicity, so it needs control it. [0003] At present, the commonly used detection method for thioglycolic acid is high performance liquid chromatography, and there are also reports using ion chromatography, thin layer chromatography, etc. for detection. At lower concentrations, acetic acid is oxidized or complexed by heavy metals and becomes unstable, thus affecting the accuracy of the detecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 罗会熊学武莫丽英李艳华黄芳芳
Owner SUNSHINE LAKE PHARM CO LTD