衍生化结合LC-MS法测定硝酸硫康唑中2种基因毒性杂质
Determination of two genotoxic impurities in sulconazole nitrate by combining derivatization with LC-MS method
郭志强 1李铁军 1孙迎基 1李佩佩 1王琦1
作者信息
- 1. 山东京卫制药有限公司,山东泰安 271000
- 折叠
摘要
针对硝酸硫康唑中硫酸烷基酯类基因毒性杂质(包括硫酸二甲酯、硫酸二乙酯),开发了方法进行检测.HILIC色谱柱(2.1 mm×50 mm,3 μm),水相为20 mmol·L-1甲酸铵溶液-甲酸(1 000∶1),有机相为乙腈,水相-有机相(10∶90),流速0.2 mL·min-1,柱温20 ℃;采用多反应监测(MRM)模式定量检测.探讨了温度、时间对衍生化的影响.该方法硫酸二甲酯、硫酸二乙酯线性相关系数分别为0.999 7和0.998 9,回收率分别为80.3％～102.3％、90.3％～100.0％,操作简单,满足定量分析要求.
Abstract
An analytical method was established for the determination of alkyl sulfate esters genotoxic im-purities in sulconazole nitrate,including dimethyl sulfate and diethyl sulfate.The separation was per-formed on an HILIC column(2.1 mm×50 mm,3 μm)utilizing the aqueous phase of 20 mmol·L-1 ammo-nium formate solution-formic acid(1 000∶1)and the organic phase of acetonitrile with isocratic elution(10∶90)at the flow rate of 0.2 mL·min-1.The column temperature was set at 20 ℃.Multiple reaction monitoring(MRM)mode was performed on quantitative determination.Effects of temperature and time for derivatization were investigated.Under the conditions,the linear correlation coefficient of dimethyl sulfate and diethyl sulfate were 0.999 7 and 0.998 9,respectively.And the recovery were 80.3％—102.3％and 90.3％—100.0％,respectively.The operation is simple and meets the requirements of quantitative analysis.
关键词
硝酸硫康唑/衍生化/液质联用/基因毒性杂质/硫酸二甲酯/硫酸二乙酯Key words
sulconazole nitrate/derivatization/LC-MS/genotoxic impurities/dimethyl sulfate/diethyl sulfate引用本文复制引用
出版年
2025
NETL
NSTL
万方数据