目的为满足药品监管的需要,快速高效检测固体药物制剂中的残留溶剂,建立一种气相色谱-质谱联用方法(GC-MS),可定性定量分析药品中50种残留溶剂。方法该方法利用选择离子监测(SIM)技术,可同时检测固体药物制剂中的苯、四氯化碳、1,2-二氯乙烷、1,1,1-三氯乙烷、乙腈、氯苯、丙酮等50种残留溶剂。结果 50种残留溶剂均具有较好的线性关系,相关系数0.997 5以上;高、中、低3个浓度的平均回收率为88.8%~109.8%,相对标准偏差(RSDs)小于11.6%,50种残留溶剂的检出限(LOD,S/N≥3)为0.000 03~0.3μg·mL-1,定量限(LOQ,S/N≥10)为0.000 09~1μg·mL-1。结论该方法操作简单、快速、灵敏、准确,适用于片剂、胶囊等固体药物制剂中的多种未知残留溶剂的同时检测。 OBJECTIVE To meet the needs of drug regulation, the residual solvents in solid pharmaceutical preparations were rapidly and efficiently detected by gas chromatography-mass spectrometry (GC-MS), and 50 kinds of residual solvents were qualitatively and quantitatively analyzed. Methods This method, using selective ion monitoring (SIM), can simultaneously detect benzene, carbon tetrachloride, 1,2-dichloroethane, 1,1,1-trichloroethane, acetonitrile, Benzene, acetone and other 50 kinds of residual solvents. Results The results showed that all the 50 residual solvents had a good linearity with a correlation coefficient of 0.997 5. The average recoveries of the three concentrations were 88.8% -109.8%, RSDs were less than 11.6% and 50% The limit of detection (LOD, S / N≥3) of residual solvents was 0.0003-0.3μg · mL-1, and the limit of quantification (LOQ, S / N≥10) was 0.0009-1μg · mL-1. Conclusion The method is simple, rapid, sensitive and accurate. It is suitable for the simultaneous detection of many unknown residual solvents in solid pharmaceutical preparations such as tablets and capsules.