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Method for detecting genotoxic impurities in AL58805 bulk drug or medicinal preparation by using high-performance liquid chromatography

An AL58805, high-performance liquid chromatography technology, applied in the field of analysis of genotoxic impurities, can solve the problems of high price, restricted promotion and use, etc., and achieve the effects of strong specificity, high sensitivity and low detection cost

Active Publication Date: 2017-08-11
常州佳德医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, although the mass spectrometer is a high-sensitivity general-purpose detector, its high price limits its popularization and use

Method used

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  • Method for detecting genotoxic impurities in AL58805 bulk drug or medicinal preparation by using high-performance liquid chromatography
  • Method for detecting genotoxic impurities in AL58805 bulk drug or medicinal preparation by using high-performance liquid chromatography
  • Method for detecting genotoxic impurities in AL58805 bulk drug or medicinal preparation by using high-performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Preparation of standard stock solution

[0042] Accurately weigh an appropriate amount of methyl p-toluenesulfonate and ethyl p-toluenesulfonate reference substance respectively, add acetonitrile to dissolve and dilute to make a solution containing about 1mg in each 1mL as a standard stock solution, and then use acetonitrile-water (50:50V / V) gradually diluted to the desired concentration.

[0043] 2. Liquid Chromatography Conditions

[0044] The chromatographic column is InertSustain C18 (4.6×250mm, 5μm); the mobile phase is 15mmol / L phosphoric acid aqueous solution-acetonitrile

[0045] (50:50V / V); the detection wavelength is 225nm; the flow rate is 1mL / min; the column temperature is 35°C; the injection volume is 20μL; the elution time is 18min.

[0046] 3. Sample pretreatment method

[0047] Take about 100mg of the AL58805 test sample, put it in a 10mL measuring bottle, add an appropriate amount of acetonitrile-water (50:50V / V) to dissolve, adjust the pH to 9 w...

Embodiment 2

[0077] 1, the preparation of standard stock solution is identical with embodiment 1;

[0078] 2. In liquid chromatography conditions: the mobile phase is 5mmol / L phosphoric acid aqueous solution-acetonitrile (50:50V / V); the rest are the same as in Example 1.

[0079] 3. Sample pretreatment: the same as in Example 1.

[0080] 4, methodological verification is identical with embodiment 1, and the result shows, the average rate of recovery of methyl p-toluenesulfonate (the standard in Pharmacopoeia is 80-115%) is 89.0%, and RSD is 1.6%, and the average recovery rate of ethyl p-toluenesulfonate Rate (standard is 80-115% in Pharmacopoeia) is 101.7%, and RSD is 2.3%, and the accuracy that this method detects methyl p-toluenesulfonate, ethyl p-toluenesulfonate is good.

Embodiment 3

[0082] 1, the preparation of standard stock solution is identical with embodiment 1;

[0083] 2. The mobile phase in the liquid chromatography conditions is 50mmol / L phosphoric acid aqueous solution-acetonitrile (50:50V / V); the rest are the same as in Example 1.

[0084] 3. Sample pretreatment: the same as in Example 1.

[0085] 4, methodological verification is identical with embodiment 1, and the result shows, the average recovery rate of methyl p-toluenesulfonate is 93.1%, and RSD is 1.7%, and the average recovery rate of ethyl p-toluenesulfonate is 102.1%, and RSD is 2.7%, The method has good accuracy in detecting methyl p-toluenesulfonate and ethyl p-toluenesulfonate.

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Abstract

The invention relates to a method for detecting genotoxic impurities in an AL58805 bulk drug or medicinal preparation by using high-performance liquid chromatography. The method is directed at methyl p-toluenesulfonate (MPTS) and ethyl p-toluenesulfonate (EPTS); a sample undergoes pre-treatment at first; and then high-performance liquid chromatography is employed for determination, wherein a C18 chromatographic column is employed; detection wavelength is 225 nm; an aqueous acetonitrile-phosphoric acid solution is used as a mobile phase; flow velocity is 0.8 to 1.2 mL / min; column temperature is 30 to 40 DEG C; a sample size is 20 [mu]L; and elution time is 18 min. Results show that the detection limit of MPTS is 0.3 ppm and the limit of quantitation of MPTS is 1 ppm; and the detection limit of EPTS is 0.5 ppm and the limit of quantitation of EPTS is 1.4 ppm. The method has the advantages of good specificity, simple operation, high sensitivity and accurate results and is applicable to determination of MPTS and EPTS in AL58805.

Description

technical field [0001] The present invention relates to an analysis method of genotoxic impurities in AL58805 bulk medicine or pharmaceutical preparations, in particular to a method for separating genotoxic impurities methyl p-toluenesulfonate and ethyl p-toluenesulfonate in AL58805 by high performance liquid chromatography and quantitative methods. Background technique [0002] AL58805 is a class of new drug developed by Nanjing Aidecheng Pharmaceutical Technology Co., Ltd. It is a new type of PI3K / mTor dual-target kinase inhibitor screened by computer-aided drug design technology, and has completely independent intellectual property rights. The previous research results show that AL58805 is an excellent anti-tumor drug with a unique target, obvious anti-tumor effect, and low toxic and side effects. It has been proved to have obvious anti-tumor activity, therefore, it will have unique advantages in clinical treatment of tumors after being developed into a new drug. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14G01N2030/146
Inventor 朱小华
Owner 常州佳德医药科技有限公司
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