论文部分内容阅读
目的:建立测定齐拉西酮残留溶剂的顶空毛细管气相色谱法。方法:采用程序升温法,FID检测器,色谱柱为DB-624毛细管柱(30.0m×0.53mm,df=3.0μm),载气为氮气,进样口温度为250℃,柱温50℃,保持8min,以10℃/min的速度升到150℃,再以50℃/min的速度升到200℃保持6min,检测器温度2 50℃,顶空温度为1 00℃。结果:在该条件下甲醇、乙醇、丙酮、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、甲苯及二甲苯的浓度与色谱峰面积线性关系良好,相关系数均大于0.999,平均回收率在95%-105%之间,RSD﹤3%,符合药典规定。结论:所用顶空气相色谱法简便、准确、灵敏度高,适用于本药物残留溶剂的测定。
Objective: To establish a capillary gas chromatographic method for the determination of ziprasidone residual solvent. Methods: A temperature-programmed and FID detector was used. The column was DB-624 capillary column (30.0m × 0.53mm, df = 3.0μm). The carrier gas was nitrogen and the inlet temperature was 250 ℃. Maintained 8min to 10 ℃ / min speed rose to 150 ℃, then 50 ℃ / min speed rose to 200 ℃ for 6min, the detector temperature of 250 ℃, the head space temperature of 100 ℃. Results: Under these conditions, the concentrations of methanol, ethanol, acetone, acetonitrile, methylene chloride, n-hexane, ethyl acetate, tetrahydrofuran, toluene and xylene had good linear relationship with the chromatographic peak area, the correlation coefficients were all above 0.999. 95% -105%, RSD <3%, in line with the provisions of the Pharmacopoeia. Conclusion: The headspace gas chromatography is simple, accurate and sensitive. It is suitable for the determination of residual solvents in this drug.