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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 GC method for the determination of 11 residual solvents in anastrozole and confirm the presence of residual solvents in the sample by GC-MS. Methods The headspace sampling was performed on a DB-624 (6% cyanopropyl phenyl-94% dimethyl polysiloxane) quartz capillary column. The column temperature was 40 ℃ and maintained for 7 min at 10 ℃ · min-1 rate rose to 180 ℃, maintained 4 min, dimethylformamide as a solvent. Results The analytes were well separated. The peak area showed a good linear relationship with the concentration. The precision and recovery were good. The residual solvents detected in the samples were confirmed by GC-MS. Conclusion This method can be used for the determination of residual solvent in Anastrozole API.