毛细管气相色谱法测定奋乃静和盐酸氟奋乃静原料药中的甲苯残留量

目的:建立一种同时测定奋乃静和盐酸氟奋乃静原料药中甲苯残留量的方法。方法:采用毛细管气相色谱法。毛细管柱为HP-5,载气为N2,检测器为氢火焰离子化检测器,柱温为50℃,进样口温度为200℃,检测器温度为250℃,分流比为10∶1,溶剂为二甲亚砜,内标物为异辛烷,以内标法计算残留溶剂甲苯的含量。结果:甲苯检测质量浓度在9.266¹11.192μg/ml范围内同甲苯与内标峰面积的比值呈良好的线性关系(r=0.999 4);检测限和定量限分别为0.593μg/ml和1.464μg/ml;精密度、稳定性、重复性试验的RSD≤5.79%;奋乃静和盐酸氟奋乃静中的平均加样回收率分别为104.77%(RSD=3.39%,n=9)和108.31%(RSD=1.09%,n=9);两种原料药各3批样品检测甲苯残留量均未超标。结论:该方法结果准确、可靠,可用于奋乃静和盐酸氟奋乃静原料药中甲苯残留量的测定。

Determination of Residual Methylbenzene in Perphenazine and Fluphenazine Hydrochloride by Capillary GC

OBJECTIVE：To establish the method for simultaneous determination of residual methylbenzene in perphenazine and perphenazine hydrochloride. METHODS：Capillary GC method was adopted. HP-5 capillary column was used with the column temperature of 50 ℃. Using N2 as carrier gas,FID was used as detector with temperature of 250 ℃. The temperature of injector was 200 ℃ and split ratio was 10 ∶ 1. Using dimethyl sulfoxide as solvent and isooctane as internal standard,the content of residual methylbenzene was calculated by internal standard method. RESULTS：The linear range of methylbenzene was 9.266-111.192 μg/ml（r=0.999 4）;the limits of detection and quantitation were 0.593 μg/ml and 1.464 μg/ml;RSDs of precision,stability and reproducibility tests were all lower than 5.79%. Average recovery of perphenazine and perphenazine hydrochloride were 104.77%（RSD=3.39%,n=9）and 108.31%（RSD=1.09%,n=9）,respectively. The contents of residual methylbenzene in 3 batches of perphenazine or perphenazine hydrochloride were all within the standard limit. CONCLUSIONS：The method is accurate and reliable,and can be used for the determination of residual methylbenzene in perphenazine and perphenazine hydrochloride.