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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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UHPLC-MS法测定2种硫酸氢氯吡格雷晶型中的基因毒性杂质对甲苯磺酸甲酯

Determination of genotoxic impurity methyl p-toluenesulfonate in two kinds of crystal forms of clopidogrel hydrogen sulfate

作者(英文):
分类号:R917
出版年·卷·期(页码):2017,37 (11):1994-1999
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立超高效液相色谱-三重四极杆质谱联用法(UHPLC-MS)测定2种硫酸氢氯吡格雷晶型(Ⅰ型和Ⅱ型)中基因毒性杂质对甲苯磺酸甲酯。方法:采用Zorbax Extend C18(2.1 mm×50 mm,1.8 μm)色谱柱,以0.1%甲酸水溶液为流动相A,0.1%甲酸甲醇溶液为流动相B,梯度洗脱,流速为0.4 mL·min-1,电喷雾(ESI)正离子检测模式,采用多反应监测(MRM)扫描模式,选择m/z 187→91作为定量离子对,m/z 187→155作为定性离子对。结果:对甲苯磺酸甲酯质量浓度在1.0~200 ng·mL-1范围内线性关系良好(r=0.999 9);检测限为0.5 ng·mL-1;定量限为1.0 ng·mL-1;Ⅰ型晶型和Ⅱ型晶型的加样回收率分别为97.7%和97.9%(n=9),RSD分别为1.5%和1.5%;4℃控温条件下供试品溶液在48 h内稳定性良好(RSD=1.6%);2种晶型各3批样品中均未检出对甲苯磺酸甲酯。结论:本方法结果可靠,可以用于硫酸氢氯吡格雷原料中对甲苯磺酸甲酯的检测。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To determine genotoxic impurity methyl p-toluenesulfonate in two kinds of crystal forms(crystal form I and crystal form Ⅱ) of clopidogrel hydrogen sulfate by UHPLC-MS;Methods: The separation was performed on a Zorbax Extend C18 column(2.1 mm×50 mm, 1.8 μm) with the mobile phase consisting of 0.1% formic acid aqueous solution(mobile phase A) and 0.1% formic acid methanol(mobile phase B) by gradient elution at a flow rate of 0.4 mL·min-1.Multiple reaction monitoring(MRM) was performed on a triple quadrupole mass spectrometer equipped with a ESI source in the positive mode, selecting m/z 187→91 as the quantitative ion pair and m/z 187→155 as qualitative ion pair.Results: The calibration curve was in a good linearity within the range of 1.0-200 ng·mL-1(r=0.999 9).The limit of detection was 0.5 ng·mL-1.The limit of quantification was 1.0 ng·mL-1.The spike recovery of the two crystal forms were 97.7% and 97.9%(n=9), with RSD of 1.5% and 1.5%, respectively.The sample solution was stable under 4℃ within 48 hours(RSD=1.6%).Methyl p-toluenesulfonate was not detected in sample solutions of two crystal forms.Conclusion: The method is accurate and reliable to determine methyl p-toluenesulfonate in clopidogrel hydrogen sulfate substance.

-----参考文献:---------------------------------------------------------------------------------------

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