Method used for measuring (E)3, 4, 5-triethoxy cinnamoyl chloride with LC-MS/MS

A technology of trimethoxycinnamon and namoyl, which can be used in measurement devices, instruments, scientific instruments, etc., can solve problems such as difficult detection limit requirements, and achieve the effects of good stability, strong specificity and high recovery rate.

Inactive Publication Date: 2019-01-01
中南粮油食品科学研究院有限公司 +1
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  • Application Information

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Problems solved by technology

[0029] In order to solve the deficiency that (E) 3,4,5-trimethoxycinnamoyl chloride impurity test method is difficult to reach the detection limit requirement in existing cinepazide, the present invention innovatively provides a kind of LC-MS/MS method to measure (

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  • Method used for measuring (E)3, 4, 5-triethoxy cinnamoyl chloride with LC-MS/MS
  • Method used for measuring (E)3, 4, 5-triethoxy cinnamoyl chloride with LC-MS/MS
  • Method used for measuring (E)3, 4, 5-triethoxy cinnamoyl chloride with LC-MS/MS

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Embodiment Construction

[0063] 1 Instruments and reagents

[0064] 1.1 Instrument

[0065] Liquid chromatography-tandem mass spectrometer: Agilent 1290-6460, charged spray ion source, equipped with Agilent Poroshell 120EC-C18 (100×2.1mm, 2.7μm) chromatographic column, BYK nitrogen generator.

[0066] 1.2 Reagents

[0067] Methanol (chromatographically pure, Merck, Germany); formic acid (chromatographically pure, Sinopharm Group); ethylenediamine (excellent grade, Sinopharm Group); ultrapure water (18.25MΩ×cm, Zhongwo Water); reference substance (E ) 3,4,5-trimethoxycinnamoyl chloride (purity ≥ 99%, provided by Gu Chuan Pharmaceutical Technology (Hunan) Co., Ltd.); , provided by Guchuan Pharmaceutical Technology (Hunan) Co., Ltd.); sample batch numbers (20170901, 20170902, 2017090, provided by Guchuan Pharmaceutical Technology (Hunan) Co., Ltd.).

[0068] 2 Methods and results

[0069] 2.1 Detection conditions

[0070] 2.1.1 Chromatographic conditions Mobile phase: Methanol-0.1% formic acid (V / V,...

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Abstract

The invention belongs to the technical field of medicine impurity analysis, and more specifically discloses a method used for measuring (E)3, 4, 5-triethoxy cinnamoyl chloride with LC-MS/MS. Accordingto the method, the method is invented based on the principle that (E)3, 4, 5-triethoxy cinnamoyl chloride is capable of reacting with diethylamine to generate stable compound (E) N, N-dimethyl-3, 4,5-triethoxy cinnamamide. A derivatization product is subjected to liquid chromatography tandem mass spectrometry analysis, and the conditions are as following: chromatographic column Agilent Poroshell120 EC-C18(100*2.1mm, 2.7<mu>m); mobile phase methanol-0.1% formic acid (V/V, 50:50); flow speed 0.4ml/min; column temperature 35 DEG C; sample introduction volume 5<mu>l; ion source electrospray iontrap (ESI); detection method positive ion multi-reaction monitoring mode; the monitoring ion pairs of (E) N, N-dimethyl-3, 4, 5-triethoxy cinnamamide are m/s 294.0/221.0 and 294.0/190.0. The method is high in specificity, low in detection limit, high in stability, high in recovery rate, and can be used for quality control of impurity (E)3, 4, 5-triethoxy cinnamoyl chloride in cinepazide maleate production process.

Description

technical field [0001] The invention belongs to the field of drug impurity analysis, and specifically discloses an analysis method for impurity (E) 3,4,5-trimethoxycinnamoyl chloride in cinepazide maleate. Background technique [0002] The chemical name of cinepazide maleate is (E)1-[(pyrrolidinecarbonyl)methyl]-4-(3,4,5-trimethoxycinnamoyl)piperazine maleate, commercial product Kelinao, a piperazine calcium antagonist [1] , has a variety of pharmacological effects, such as the synergistic effect of adenosine [2] , Vasodilator effect [3] , improve blood rheology [4] , widely used in the treatment of cardiovascular and cerebrovascular diseases [5～9] , first produced by the French Sanofi-Anentis company in 1970, and widely used in developed countries such as Europe and Japan, and launched in China in 2002 [1] . [0003] There are four main synthetic routes of cinepazide maleate, and (E)3,4,5-trimethoxycinnamoyl chloride is used as the raw material for the intermediate re...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 何攀彭湘林张源泉谢婷婷陈渠玲莫兵聂蓬勃刘明闫东阁李枣枣
Owner 中南粮油食品科学研究院有限公司
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