气相色谱法测定齐拉西酮冻干粉针剂中叔丁醇残留量

摘要

Objective To establish the gas chromatography method to determine the tert-butyl alcohol residue in Ziprasidone Freeze-Dried Powder Injection. Methods PEG-20M capillary column ( 30 m × 0. 32 mm, 0. 50 μm ) was used with external standard measure-ment. The detection limits, standard curve, recovery rate and stability of the reference substance of Tert-butyl alcohol was detected by gas chromatography, and the residue of Tert-butyl in different batches of Ziprasidone freeze-dried powder injection was investigated. Results The mass concentration of tert-butyl alcohol in the range of 20-400 μg/mL had good linear relationship with the peak area ( r=0. 999 3 ) , the detection limit was 0. 010 μg/mL, the recovery was 97. 15%, 101. 54%, 101. 86 %, and the precision and re-covery RSD ﹤ 1. 5%. Conclusion This method is sensitive with good reproducibility and good system suitability, and is suitable for the determination of the tert-butyl alcohol residue in Ziprasidone Freeze-Dried Powder Injection.%目的：建立测定齐拉西酮冻干粉针剂中叔丁醇残留量的气相色谱法。方法采用PEG－20M毛细管柱（30 m ×0.32 mm，0.50μm），采用外标法定量，考察叔丁醇对照品的检测限、标准曲线、加样回收率及稳定性，并对不同批次的齐拉西酮冻干针剂中叔丁醇残留量进行考察。结果叔丁醇质量浓度在20~400μg/mL范围内与峰面积线性关系良好( r=0.9993)，最低检出限为0.010μg/mL；高、中、低3种质量浓度的加样回收率为97.15%，101.54%，101.86%，精密度及回收率的 RSD均小于1.5%。结论该方法灵敏，重现性良好，系统适用性良好，可用于测定齐拉西酮冻干粉针剂中叔丁醇残留量。