GC-MS/SIM法测定盐酸鲁拉西酮片中甲磺酸酯类物质残留量

摘要

建立了气相色谱-质谱/选择离子监测法(GC-MS/SIM),检测盐酸鲁拉西酮片中甲磺酸酯类物质残留量.使用DB-624毛细管色谱柱(30m×0.32mm×1.8μm)实现了甲磺酸酯的分离,对提取溶剂、起始柱温、分流比等条件参数进行了优化.在选择离子监测模式(SIM)下,选取适宜的特征离子,进行定性定量分析.结果表明,目标物在0.01~0.40mg/L范围内线性关系均良好,线性相关系数(R2)均大于0.999;检出限、定量限均分别为0.003mg/L、0.01mg/L;在0.16、0.20、0.24mg/L三个加标浓度下,平均回收率为88.43% ~104.15%,相对标准偏差为0.97% ~1.82%.该方法精密度良好,操作简便快速、准确可靠、灵敏度高,适用于盐酸鲁拉西酮片中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯残留的同时检测.%Mesylate esters were separated with the DB-624 capillary column(30m×0.32mm×1.8μm) under optimized pretreatment conditions and GC parameters including the extraction solvent of samples, the initial column oven temperature and the split ratio of GC.The selected ion monitor(SIM)mode was used for the qualitative and quantitative analysis by the selection of characteristic ions of mesylate esters. The results were validated that the calibration curves had good correlation coefficients(R2>0.999)in the range of 0.01 -0.40mg/L. The limits of detection and quantitation for all the mesylate esters were 0.003mg/L and 0.01mg/L,respectively. The mean recoveries for mesylate esters at three spiked levels (0.16,0.20,0.24mg/L)were 88.43% -104.15% with relative standard deviations of 0.97% -1.82%and with good precisions. The method is simple,rapid,accurate,reliable,highly sensitive.