摘要
目的测定左卡尼汀中遗传毒性物质S-环氧氯丙烷的含量。方法采用气相色谱-质谱联用(GC-MS)法。色谱柱为Agilent HP-5ms毛细管柱;程序升温,进样口温度200℃;柱流量为1.0 mL·min^(-1);分流进样,分流比为5∶1;载气为高纯氦气;检测器为质谱检测器;离子化方式为EI;离子化电压为70 eV;离子源温度为230℃;传输线温度为260℃;溶剂延迟时间为2.8 min;检测方式为选择离子扫描模式(SIM);进样量为1μL。结果空白溶剂与左卡尼汀均不干扰S-环氧氯丙烷的检测,其在55.11~220.44 ng·mL^(-1)与峰面积呈良好的线性关系(r=0.996);S-环氧氯丙烷平均回收率均大于100.0%,RSD均小于8.6%(n=3)。结论该方法简便、准确、灵敏,可用于左卡尼汀原料药中遗传毒性杂质S-环氧氯丙烷的检测。
Objective To determine the genotoxic substance S-epichlorohydrin in levocarnitine.Method Gas chromatography-mass spectrometry(GC-MS)method was used.The chromatographic column was Agilent HP-5ms capillary column with programmed heating.The inlet temperature was 200℃;the column flow rate was 1.0 mL·min^(-1);split injection was used as the sampling method,and the split ratio was 5∶1;the carrier gas was high purity helium;a mass spectrometer detector was set;the ionization method was EI,with the ionization voltage at 70 eV;the ion source temperature at 230℃;the temperature of the transmission line at 260℃;and the solvent delay time at 2.8 min.The detection method was selected ion scanning mode with the injection volume of 1μL.Results Neither the blank solvent nor levocarnitine interfered with the detection of S-epichlorohydrin.A good linearity was found at 55.11~220.44 ng·mL^(-1)(r=0.996).The average recovery of S-epichlorohydrin was more than 100.0%,and the RSD was less than 8.6%(n=3).Conclusion The method is simple,accurate and sensitive,and can be used for the detection of genotoxic impurity S-epichlorohydrin in the raw material of levocarnitine.
作者
王淋
李雪
朴惠顺
李敏
段成军
WANG Lin;LI Xue;PIAO Hui-shun;LI Min;DUAN Cheng-jun(School of Pharmacy,Yanbian University,Yanji Jilin 133000;Jilin Broadwell Pharmaceutical Co.Ltd.,Changchun 130000)
出处
《中南药学》
CAS
2021年第4期727-729,共3页
Central South Pharmacy
