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A kind of high performance liquid chromatography determination method of p-carboxybenzenesulfonamide

A technology of carboxybenzenesulfonamide and high-performance liquid chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of many by-products, bad environment of waste liquid, impact, etc., and achieve fast analysis speed and less sample consumption , the effect of high sensitivity

Inactive Publication Date: 2016-04-06
CHINA UNIV OF MINING & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the preparation of p-carboxybenzenesulfonamide is obtained through the oxidation of p-toluenesulfonamide. The traditional oxidant is not only expensive, but also has many by-products, and the discharged waste liquid also has a bad impact on the environment. Looking for a new "green" It is necessary to use an efficient and convenient analytical method capable of qualitative and quantitative detection of p-carboxybenzenesulfonamide to evaluate it.
There is no report on the qualitative and quantitative analysis method of carboxylbenzenesulfonamide in the literature of the prior art, and thin-layer chromatography can't be quantified in conventional determination method, and gas chromatography can't detect that this class of p-carboxybenzenesulfonamide has high boiling point, large polarity, and is difficult to gas. compound

Method used

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  • A kind of high performance liquid chromatography determination method of p-carboxybenzenesulfonamide
  • A kind of high performance liquid chromatography determination method of p-carboxybenzenesulfonamide
  • A kind of high performance liquid chromatography determination method of p-carboxybenzenesulfonamide

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preparation example Construction

[0040] The preparation method of reference substance solution and sample solution is as follows:

[0041]Preparation of reference substance solution: Accurately weigh a certain amount of dry pure p-carboxybenzenesulfonamide as a reference substance, dissolve it in a solvent, and ultrasonically treat it at 60°C for 10 minutes to prepare a solution containing 0-100 μg of p-carboxybenzenesulfonamide per 1 mL. A series of solutions, the series of solutions of p-carboxybenzenesulfonamide are 0 μg / mL, 20 μg / mL, 40 μg / mL, 60 μg / mL, 80 μg / mL and 100 μg / mL, after filtering through a 0.15-0.3pm microporous membrane As a reference solution;

[0042] Preparation of sample solution: Take the oxidized product of p-toluenesulfonamide, wash with water, filter and dry, weigh 0.0375g accurately, dissolve it with a solvent, and ultrasonically treat it at 60°C for 10min, then dilute to 25mL with a solvent , to obtain the test solution; accurately pipette 1mL of the test solution, use a solvent t...

Embodiment 1

[0060] Embodiment 1, a kind of high-performance liquid chromatography determination method of p-carboxybenzenesulfonamide, the method adopts high-performance liquid chromatography to measure the yield and selectivity of p-toluenesulfonamide oxidation synthesis p-carboxybenzenesulfonamide, comprising the following steps:

[0061] (1) Chromatographic conditions: the chromatographic column uses octadecylsilane bonded silica gel as a filler; the 0.02mol / L sodium dihydrogen phosphate buffer solution with pH=2.0 is used as the A mobile phase, and acetonitrile is used as the B mobile phase, wherein A The ratio of mobile phase to mobile phase B is 60:40, the isocratic elution method is adopted, the flow rate of the mobile phase is 1mL / min, the detection wavelength is 230nm, the column temperature is 25°C, and the injection volume is 20μL / min;

[0062] (2) Determination: the p-toluenesulfonamide oxidation product is injected into a high-performance liquid chromatograph, and is measured ...

Embodiment 2

[0064] Embodiment 2, a high-performance liquid chromatography determination method of p-carboxybenzenesulfonamide, the method adopts high-performance liquid chromatography to determine the yield and selectivity of p-toluenesulfonamide oxidation synthesis p-carboxybenzenesulfonamide, comprising the following steps:

[0065] (1) Chromatographic conditions: the chromatographic column uses octadecylsilane bonded silica gel as a filler; the 0.001mol / L sodium dihydrogen phosphate buffer solution with pH=4.0 is used as the A mobile phase, and acetonitrile is used as the B mobile phase, wherein A The ratio of mobile phase to mobile phase B is 70:30, using the isocratic elution method, the flow rate of the mobile phase is 1mL / min, the detection wavelength is 230nm, the column temperature is 25°C, and the injection volume is 20μL / min;

[0066] (2) Determination: the p-toluenesulfonamide oxidation product is injected into a high-performance liquid chromatograph, and is measured by the chr...

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Abstract

The invention discloses a high-performance liquid chromatography determination method for p-carboxybenzenesulfonamide, which belongs to the high-performance liquid chromatography determination method. The method adopts Agilent1200 type high-performance liquid chromatography, and the chromatographic conditions are as follows: the chromatographic column uses a C18 reverse-phase column, the sodium dihydrogen phosphate buffer solution is used as the A mobile phase, and acetonitrile is used as the B mobile phase, and an isocratic elution method is adopted. The flow rate of the phase is 1mL / min, the detection wavelength is 230nm, the column temperature is 25°C, and the injection volume is 20μL / min; the oxidation product of p-toluenesulfonamide is injected into the liquid chromatograph, and according to the retention time and peak area At the same time, the qualitative and quantitative detection of p-toluenesulfonamide and p-carboxybenzenesulfonamide was further analyzed to obtain the yield and selectivity of p-toluenesulfonamide oxidation to p-carboxybenzenesulfonamide. The method of the invention has high accuracy, high sensitivity, quickness, convenience and comprehensive analysis, and provides a powerful detection tool for process optimization of p-carboxybenzenesulfonamide.

Description

technical field [0001] The invention relates to a liquid chromatography determination method, in particular to a high performance liquid chromatography determination method of p-carboxybenzenesulfonamide. Background technique [0002] p-Carboxybenzenesulfonamide is an important pharmaceutical intermediate, which is used to synthesize probenecid, harazone, etc. Its sodium salt can be used as an inhibitor of carbonic anhydrase, and its development and utilization are very promising. Generally, the preparation of p-carboxybenzenesulfonamide is obtained through the oxidation of p-toluenesulfonamide. The traditional oxidant is not only expensive, but also has many by-products, and the discharged waste liquid also has a bad impact on the environment. Looking for a new "green" It is very necessary to have an oxidation method, and it is very important to evaluate it with an efficient and convenient analytical method capable of qualitative and quantitative detection of p-carboxybenze...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 梁静杨会会毛声义孟献梁刘亚军
Owner CHINA UNIV OF MINING & TECH