针对药品恩诺沙星生产过程中易生成的毒性物质硫酸二甲酯,建立了气质联用仪测定硫酸二甲酯的方法.用Agilent HP-5MS色谱柱(30.0m×0.25mm×0.25μm),采用选择离子扫描模式(SIM)和程序升温法(初始温度50℃,保持2 min,以10℃/min升温至90℃,保持1 min,再以9℃/min升温至180℃).结果表明,硫酸二甲酯的检测限(LOD,S/N≥3)为0.002μg/mL;在0.01~1.00μg/mL浓度范围内呈线性关系,相关系数在0.999以上;实际样品检测的加标回收率均在83.50%~113.20%之间.该法准确简便,可应用于实际检测. A method for the determination of dimethyl sulfate by gas chromatography-mass spectrometry (GC-MS) was developed for the toxicity-prone substance dimethyl sulfate in the process of enrofloxacin production.Using Agilent HP-5MS column (30.0m × 0.25mm × 0.25μm) (SIM) and temperature programmed method (initial temperature of 50 ° C for 2 min, temperature of 10 ° C / min to 90 ° C for 1 min and temperature of 9 ° C / min to 180 ° C) .Results The results showed that the limit of detection (LOD, S / N≥3) of dimethyl sulfate was 0.002μg / mL, the linear range was 0.01 ~ 1.00μg / mL, the correlation coefficient was above 0.999. The recoveries are between 83.50% ~ 113.20% .The method is accurate and convenient, can be applied to the actual test.