气相色谱-质谱法同时分析固体药物制剂中50种残留溶剂

Simultaneous Determination of 50 Residual Solvents in Solid Drug Preparations by GC-MS

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0．9975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0．00003～0．3μg·mL^-1，定量限（LOQ，S/N≥10）为0．00009～1μg·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 develop an analytical method for determination of unknown residual solvents in solid drug products by GC-MS in order to meet the need of supervision. METHODS Fifty residual solvents including benzene, carbontetrachloride, 1,2-di chloroethane, 1,1,1-trichloroethane, acetonitrile, chlorobenzene, acetone, etc, were determined by GC/MS using selected ion monito ring （SIM） mode. RESULTS Good linearity was obtained with correlation coefficients of more than 0. 997 5 for all the solvents. The av erage recoveries of the quality control samples at low, middle and high concentrations were from 88. 8% to 109. 8% and the relative standard deviations （RSDs） were lower than 11. 6%. The limits of detection （LODs） were in the range of 0. 000 03 -0. 3 μg . mL^-1 , while the limits of quantitation （LOQs） were in the range of 0. 000 09 - 1μg . mL^-1. CONCLUSION The method is simple, rapid, sensitive and accu rate, and can be used for the simultaneous determination of 50 residual solvents in solid preparations such as tablets and capsules.