A method for the simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid

A technology of maleic anhydride and thiomalic acid, applied in the field of simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid, can solve the problem of thiomalic acid, thiourea and maleic anhydride determination Inapplicable and other problems, to achieve the effect of good accuracy performance, easy popularization and promotion, and simple processing process

Active Publication Date: 2021-11-12
HENGSHENG TECH R&D CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above two methods are suitable for the determination of dimercaptosuccinic acid related substances, they are not suitable for the determination of thiomalic acid, thiourea and maleic anhydride

Method used

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  • A method for the simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid
  • A method for the simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid
  • A method for the simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0052] A method for quantitatively analyzing maleic anhydride, thiourea and thiomalic acid simultaneously, comprising the steps of:

[0053] (1) Preparation of standard solution:

[0054] Weigh 0.0487g thiourea standard product, 0.0509g maleic anhydride standard product and 0.2234g thiomalic acid standard product respectively and place them in a 100mL volumetric flask; solution, the concentration of the reference standard solution is denoted as X; the reference standard solution is diluted with a solvent to make a standard solution with a concentration of 0.01X, 0.02X, 0.04X, 0.1X, 0.2X, 0.5X and 1.0X;

[0055] (2) the standard solution prepared by step (1) is injected into the liquid chromatograph to measure;

[0056] Described liquid chromatograph adopts ultraviolet detector, and detection wavelength is 211nm; Chromatographic column is ZORBAX Extend-C18 liquid phase chromatographic column (150 * 4.6mm, 5 μ m); Column temperature 25 ℃; Mobile phase is methanol: aqueous phosp...

Embodiment 2

[0089] A kind of assay method of quantitative analysis maleic anhydride, thiourea raw material purity, adopt the test method established in embodiment 1, measure the purity of maleic anhydride and thiourea raw material, specifically comprise the steps:

[0090] (1) Preparation of test sample solution: accurately weigh 50 mg of maleic anhydride and 40 mg of thiourea and place them in a 100 mL volumetric flask, add deionized water to completely dissolve the solid sample, and dilute to the mark, shake well, and filter with 0.45 μm Membrane filtration promptly obtains the test sample solution;

[0091] (2) the test sample solution that step (1) obtains is injected in the high-performance liquid chromatograph, analyze, and analysis condition is:

[0092] ZORBAXSB-Aq liquid chromatography column (150 * 2.1mm, 3.5 μ m); Column temperature 35 ℃; Mobile phase is methanol-0.1% phosphoric acid aqueous solution=30:70; Flow velocity is 1.0mL / min; Detection wavelength is 211nm; The sample ...

Embodiment 3

[0096] A method for simultaneous quantitative analysis of maleic anhydride, thiourea and thiomalic acid, using the test method established in Example 1, for maleic anhydride, thiourea and thiomalic acid in the thiomalic acid preparation reaction solution The content of substitute malic acid is measured, specifically comprises the following steps:

[0097] (1) Prepare the test sample solution: accurately pipette 0.5 mL of the reaction solution prepared by thiomalic acid and place it in a 50 mL volumetric flask, add high-purity water to dilute to the mark, shake well, and filter with a 0.45 μm filter membrane to obtain the test sample solution ;

[0098] (2) Inject the test sample solution obtained in step (1) into a high-performance liquid chromatograph for analysis, and the analysis conditions are: ZORBAXExtend-C18 liquid chromatography column (150 × 4.6mm, 5 μm); column temperature 25°C; The mobile phase is methanol-0.1% phosphoric acid aqueous solution=10:90; the flow rate ...

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Abstract

The invention relates to a method for quantitatively analyzing maleic anhydride, thiourea and thiomalic acid simultaneously. The method comprises the steps of: (1) taking by weighing maleic anhydride, thiourea and thiomalic acid standard substance, preparing a standard solution; (2) taking maleic anhydride, thiourea and thiomalic acid The mixture formed is the test sample, and the test sample solution is prepared; (3) get the standard solution and the test sample solution respectively for high-performance liquid chromatography analysis, conditions: C18 liquid chromatography column, column temperature 25~45 ℃, flowing Phase methanol and phosphoric acid aqueous solution, the flow rate is 0.5-2.0mL / min, the detection wavelength of the ultraviolet detector is 200-235nm, and the content is obtained by the external standard method; the sequence of steps (1) and (2) is not limited. The method can quickly and simultaneously quantitatively analyze the contents of maleic anhydride, thiourea and thiomalic acid, and has high sensitivity, accuracy, stability and reproducibility.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for simultaneously quantitatively analyzing maleic anhydride, thiourea and thiomalic acid. Background technique [0002] Thiomalic acid is a multifunctional compound. Due to the strong reduction and chelating coordination properties of sulfhydryl groups, it has a wide range of uses. Thiomalic acid can be used as a complexometric titration masking agent, a heavy metal antidote, and can be used in Fluorescent probes are used to detect metal ions. They are raw materials for the preparation of various sulfur-containing drugs, and are also the main component of cold perm agents and additives for cleaning gold plating. They have important application values. [0003] The synthesis of thiomalic acid has been reported mainly aspartic acid method, phosphorothioate method, maleic acid method and thiourea method. Wherein the thiourea method becomes the method commonly used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74
Inventor 唐海燕张磊张笛徐红彬张懿
Owner HENGSHENG TECH R&D CO LTD
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