毛细管顶空进样法测定更昔洛韦中有机溶剂残留量

Determination of the residual organic volatile solvents in ganciclovir by capillary gas chromatography with headspace sampling

目的建立以正丁醇为内标物,测定更昔洛韦中甲醇、乙醇、丙酮和甲苯殘留量的顶空气相色谱法。方法用AgilentHP5毛细管柱(30m×0.32mm×0.25μm);载气为N2,柱流量为0.8mL/min,分流比为5:1,柱温为50℃;检测器为FID,检测器温度为250℃;Agilent7694E顶空进样器,顶空瓶加热温度为90℃,加热30min;进样口温度为200℃。结果甲醇、乙醇、丙酮和甲苯的线性范围分别为:20.23～202.3μg/mL(r=0.9995),30.05～300.5μg/mL(r=0.9992),29.82～298.2μg/mL(r=0.9993)和5.05～50.5μg/mL(r=0.9996);最低检出浓度分别为:1.95,2.52,0.18和0.12μg/mL;平均回收率分别为97.22%(RSD=2.13%),96.35%(RSD=1.65%),101.2%(RSD=3.02%)和95.45%(RSD=1.05%)。结论本法简便、灵敏、准确,适用于更昔洛韦中有机溶剂殘留量的测定。

OBJECTIVE To establish a headspace sampling GC method with n-butanol as internal standard for the determination of methanol, alcohol, acetone and toluene in ganciclovir. METHODS A Agilnet HP-5 capillary column (30m×0.32mm, 0.25 μm) was used at 50℃. N_ 2 was carrier gas at a column flow rate of 0.8mL/min, split rate was 5:1. The FID detector was used at 250℃. The Agilent 7694E headspace sampling was used at heated temperature 90℃ for 30min. The injection port temperature was 200℃.RESULTS The linear range of this method in methanol, alcohol, acetone and toluene was respectively 20.23~202.3μg/mL( r = 0.9995 ),30.05~300.5μg/mL( r =0.9992),29.82~298.2μg/mL( r =0.9993) and 5.05~50.5μg/mL( r =0.9996);The limit of detection was 1.95μg/mL,2.52μg/mL,0.18μg/mL and 0.12μg/mL respectively;the average recovery was 97.22%(RSD= 2.13% ),96.35%(RSD=1.65%),101.2%(RSD=3.02%) and 95.45%(RSD=1.05%),respectively. CONCLUSION This method is a rapid, simple and accurate procedure, which is suitable for determination of the residual organic volatile solvents in ganciclovir.