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

作　　者：郭志强 李铁军 孙迎基 李佩佩 王琦 GUO Zhiqiang;LI Tiejun∗;SUN Yingji;LI Peipei;WANG Qi(Jewim Pharmaceutical(Shandong)Co.,Ltd.,Taian 271000,Shandong,China)

机构地区：[1]山东京卫制药有限公司,山东泰安271000

出　　处：《化学工业与工程》2025年第1期106-112,共7页Chemical Industry and Engineering

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, 3μm),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。An analytical method was established for the determination of alkyl sulfate esters genotoxic impurities in sulconazole nitrate,including dimethyl sulfate and diethyl sulfate.The separation was performed on an HILIC column(2.1 mm×50 mm,3μm)utilizing the aqueous phase of 20 mmol·L^(-1) ammonium formate solution-formic acid(1000∶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 0.9997 and 0.9989,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 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]