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Method for determining purity of AE-active ester by pre-column derivatization method

A pre-column derivatization, active ester technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low results, unable to accurately reflect the quality of AE-active esters, etc., and achieves high accuracy, simple and easy methods, Avoid the effects of hydrolysis

Active Publication Date: 2020-04-17
河北合佳医药科技集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the detection methods for the purity of AE-active esters include the chemical industry standard HG / T 5150-2017, the enterprise standard Q / 0323YXH002-2018, and the literature "Reversed-phase high-performance liquid chromatography for the determination of active thioesters of aminothioxime" ("chromatography" 2003 No. 1 95) and the literature "HPLC Determination of AE-Active Ester in Cefepime Hydrochloride for Injection" ("Electronic Journal of Clinical Medicine Literature" June 2019 No. 8 1-2+4) The detection method is reverse phase chromatography to directly measure its purity, the result is low and cannot accurately reflect the quality of AE-active ester

Method used

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  • Method for determining purity of AE-active ester by pre-column derivatization method
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  • Method for determining purity of AE-active ester by pre-column derivatization method

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Embodiment 1

[0032] Embodiment 1 adopts the method for measuring the purity of AE-active ester by pre-column derivatization method of the present invention

[0033] Dissolve 0.1 g of sodium borohydride in 1000 ml of methanol to prepare a sodium borohydride solution. Take 0.3 g of AE-active ester with batch number HJE2021908156, add 10 ml of sodium borohydride solution, shake for 1 minute, and dissolve. Accurately measure 1ml of the above solution and place it in a 100ml volumetric flask, keep it in a water bath at 30°C for 1 hour, take it out and let it cool to room temperature, dilute it to the mark with a mixed solution of acetonitrile and water at a ratio of 3:2, and use it as the test solution . The chromatographic column used is Century SIL C18 BDS150mm×4.6mm×5.0μm, the detection wavelength is 254nm, and the flow rate is 1ml min -1 , the mobile phase is water (containing potassium dihydrogen phosphate 4.73g L -1 , dipotassium hydrogen phosphate 1.87g·L -1 , adjust the pH to 5.0 wi...

Embodiment 2

[0036] Embodiment 2 adopts the method for measuring the purity of AE-active ester by pre-column derivatization method of the present invention

[0037] Dissolve 0.08 g of sodium borohydride in 1000 ml of methanol to prepare a sodium borohydride solution. Take 0.3 g of AE-active ester with batch number HJE2021908156, add 10 ml of sodium borohydride solution, shake for 1 minute, and dissolve. Precisely measure 1ml of the above solution and place it in a 100ml volumetric flask, keep it in a water bath at 30°C for 1 hour, take it out and put it at room temperature, dilute to the mark with a mixed solution of acetonitrile and water at a ratio of 1:1, and use it as the test solution . The chromatographic column used is Century SIL C18BDS150mm×4.6mm×5.0μm, the detection wavelength is 254nm, and the flow rate is 1ml min -1 , the mobile phase is water (containing potassium dihydrogen phosphate 4.73g L -1 , dipotassium hydrogen phosphate 1.87g·L -1 , adjust the pH to 5.0 with phosph...

Embodiment 3

[0038] Embodiment 3 adopts the method for measuring the purity of AE-active ester by pre-column derivatization method of the present invention

[0039] Dissolve 0.12 g of sodium borohydride in 1000 ml of methanol to prepare a sodium borohydride solution. Take 0.3 g of AE-active ester with batch number HJE2021908156, add 10 ml of sodium borohydride solution, shake for 1 minute, and dissolve. Precisely measure 1ml of the above solution and place it in a 100ml volumetric flask, keep it in a water bath at 30°C for 1 hour, take it out and let it cool to room temperature, dilute it to the mark with a mixed solution of acetonitrile and water at a ratio of 9:1, and use it as the test solution . The chromatographic column used is Century SIL C18BDS150mm×4.6mm×5.0μm, the detection wavelength is 254nm, and the flow rate is 1ml min -1 , the mobile phase is water (containing potassium dihydrogen phosphate 4.73g L -1 , dipotassium hydrogen phosphate 1.87g·L -1 , adjust the pH to 5.0 wit...

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Abstract

The invention discloses a method for determining the purity of AE-active ester by a pre-column derivatization method and belongs to the technical field of pharmaceutical analysis. The preparation method comprises steps that (1) the AE-active ester is added into sodium borohydride solution, and uniform shaking is performed; (2) 1ml of the solution prepared in the step (1) is put into a 100ml volumetric flask, the solution is kept in a water bath of 30 DEG C for 1 hour, the solution is taken out, the solution is put to the room temperature, and diluting is performed to a scale by using solvent to obtain a test solution; (3) the chromatographic conditions are as follows, C18 is 150mm*4.6 mm*5.0 mu m, the detection wavelength is 254nm, the flow velocity is 1ml*min<-1>, and the mobile phase iswater-acetonitrile; and the test solution is taken, the test solution is injected into a high performance liquid chromatograph, a chromatogram is recorded, and the purity is calculated by a peak areanormalization method. The method is advantaged in that the purity of the AE-active ester is determined by adopting a pre-column derivatization method, hydrolysis during direct determination is avoided, a derivatization reagent is methanol solution of sodium borohydride, and the method is simple, easy to implement and high in accuracy.

Description

technical field [0001] The invention relates to a method for measuring the purity of AE-active ester, belonging to the technical field of drug analysis. Background technique [0002] AE-active ester (MAEM), the chemical name is 2-methoxyimino-2-(2-amino-4-thiazolyl)-(z)-thiazolium thioacetate, and its structural formula is as follows: [0003] [0004] AE-active ester is the main raw material of many semi-synthetic cephalosporin antibiotics, such as cefotaxime sodium, ceftriaxone sodium, cefetamet, cefpirome and other third and fourth-generation semi-synthetic cephalosporin antibiotics An important side chain. In recent years, cephalosporin antibiotics have been widely used due to their high efficiency, low toxicity and broad antibacterial spectrum. [0005] AE-active ester is easily hydrolyzed when it meets water due to its lively nature. At present, the detection methods for the purity of AE-active esters include the chemical industry standard HG / T 5150-2017, the ent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86G01N30/74
CPCG01N30/02G01N30/06G01N30/8634G01N30/74G01N2030/067
Inventor 刘振强刘东娜梁丙辰刘艳君孙美婷
Owner 河北合佳医药科技集团股份有限公司