气质联用法测定齐多夫定中甲磺酸甲酯和对甲苯磺酸甲酯  

Determination of Methyl Methanesulfonate and Methyl p-Toluenesulfonate in Zidovudine by Gas Chromatography-Mass Spectrometry

作　　者：郑杨杨 唐嘉怡 叶明立 车金水 陈梅兰[1] ZHENG Yang-yang;TANG Jia-yi;YE Ming-li;CHE Jin-shui;CHEN Mei-Lan(College of Biological and Environmental Engineering,Zhejiang Shuren University,Hangzhou,Zhejiang,310015,China;Thermo Fisher Scientific(China)Co.,Ltd.,Shanghai 201203,China)

机构地区：[1]浙江树人大学生物与环境工程学院,浙江杭州310015 [2]赛默飞世尔科技(中国)有限公司,上海201203

出　　处：《浙江化工》2022年第8期41-45,共5页Zhejiang Chemical Industry

摘　　要：齐多夫定生产过程中易生成毒性较大的甲磺酸甲酯和对甲苯磺酸甲酯,本文建立了气质联用法检测齐多夫定产品中甲磺酸甲酯和对甲苯磺酸甲酯的方法。实验采用Aailent DB-5色谱柱(30.0 m×250μm×0.25μm),选择离子模式。程序升温以50℃为初始温度,保持1 min,以10℃/min升至200℃并保持5 min。甲磺酸甲酯的特征离子为65、80、95、109 m/z,定量离子为80 m/z;对甲苯磺酸甲酯的特征离子为65、91、155、186 m/z,定量离子为91m/z。结果表明,该法对甲磺酸甲酯的检测限为0.01μg/mL,RSD值为6.2%,回收率为103.75%~118.72%;对甲苯磺酸甲酯的检测限为0.01μg/mL,RSD值为3.8%,回收率为101.78%~119.61%。Zidovudine is prone to generate methyl methanesulfonate and methyl p-toluenesulfonate which are more toxic in the production process.In this paper,a gas chromatography-mass spectrometry(GC-MS)method was established to detect methyl methanesulfonate and methyl p-toluenesulfonate in zidovudine products.Aailent DB-5 column(30.0 m×250μm×0.25μm)was used in the experiment in selected ion mode.The temperature was programmed to take 50°C as the initial temperature,hold for 1 min,ramp to 200°C at 10°C/min and hold for 5 min.The characteristic ions of methyl methanesulfonate are 65,80,95,109 m/z,and the quantitative ions are 80 m/z;the characteristic ions of methyl p-toluenesulfonate are 65,91,155,186 m/z,and the quantitative ions are are 91 m/z.The results showed that the detection limit of methyl methanesulfonate was 0.01μg/mL,the RSD value was 6.2%,and the recovery was 103.75%~118.72%;the detection limit of methyl p-toluenesulfonate was 0.01μg/mL,The RSD value was 3.8%,and the recovery was 101.78%~119.61%.

关 键 词：齐多夫定 气质联用 甲磺酸甲酯 对甲苯磺酸甲酯 痕量 

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