分配系数和相比的选择在HS-GC测定基因毒性杂质苯中的应用

Application of partition coefficient and phase ratio selection in determining genotoxic impurity benzene by HS-GC

目的:建立药品中基因毒性杂质苯残留量的检测方法,为药物分析中苯的检测提供方法依据。方法:采用ZB-50毛细管柱(30 m×0.53 mm×1.0μm),柱温为程序升温(起始温度40℃,保持1 min,以25℃·min^(-1)的速率升温至180℃,保持3 min);进样口200℃,氢火焰离子化检测器(FID)温度为:250℃。载气为氮气,流速2.0 mL·min^(-1),分流比为10∶1;顶空进样,顶空平衡温度90℃,平衡时间为20 min。结果:苯浓度范围在0.034~0.407μg·m L^(-1)线性关系良好(r=0.9995),平均加样回收率(n=9)为92.3%(RSD=2.4%),检测下限为11.0 ng·mL^(-1),定量下限为34.0 ng·mL^(-1),5批样品中均未检出苯。结论:所建立的方法能够较好地对药品中残留的苯进行限度测定,极大的提高苯的检测效率。

Objective:To established a method for the determination of genotoxic impurity benzene residues in drug,to provide a basis for the determination of benzene in drug analysis.Methods:A ZB-50 capillary column(30 m×0.53 mm×1.0μm)was used,the temperature program for the column was as follows:initially heated at 40℃for 1 min,increased to 180℃at a speed of 25℃·min^(-1)and lasted for 3 min.The inlet temperature was 220℃and FID detector temperature was set at 250℃.The split ratio was 10∶1 and the flow rate of the carrier gas(N2)was 2.0 m L·min^(-1).Headspace conditions were as follows:the temperature and the time of shaking for the sample were 90℃and 20 min.Results:Benzene had a good linear relationship within the concentration range of 0.034-0.407μg·m L^(-1)(r=0.9995).The average recoveries(n=9)were 92.3%(RSD=2.4%).The limit of detection was 11.0 ng·m L^(-1)and the limit ofquantification was 34.0 ng·m L^(-1).Benzene was not detected in the 5 batches of samples.Conclusion:The established method greatly improved the detection efficiency of benzene residues in pharmaceuticals.