GC和GC-MS测定阿那曲唑中的11种残留溶剂

Analysis of Eleven Residual Organic Solvent in Anastrozole by GC and GC-MS

目的建立GC测定阿那曲唑中的11种残留溶剂,用GC-MS对样品中检出的残留溶剂进行确证。方法采用顶空进样,色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱,柱温为40℃,维持7 min,以10℃·min-1速率升至180℃,维持4 min,二甲基甲酰胺为溶剂。结果被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度和回收率良好,通过GC-MS对样品中检出的残留溶剂进行了确证。结论该法可用于阿那曲唑原料药中残留溶剂的检测。

OBJECTIVE To establish a method of GC for the determination of residual solvents in anastrozole, a method of GC/MS for the verification of residual solvents in anastrozole. METHODS DB-624 capillary column through head-space sampling mode was used. The column temperature was maintained at 40 ℃ for 7 min, then was raised to 180 ℃ at the rate of 10 ℃·min^-1 and maintained at 180 ℃ for 4 min. The sample was dissolved in dimethylformamide. RESULTS The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. The residual solvents in anastrozole were confirmed by GC-MS. CONCLUSION The established method is simple and reliable, which can be used for determination of residual solvents in anastrozole.