顶空毛细管气相色谱法测定腺嘌呤原料药中5种有机溶剂残留量

目的:建立测定腺嘌呤原料药中二氯甲烷、三氯甲烷、苯、三氯乙烯和二氧六环等5种有机溶剂残留量的分析方法。方法:采用顶空毛细管气相色谱法。以1 mol/L氢氧化钠溶液溶解样品,DB-624石英毛细管为色谱柱;程序升温;进样口温度200℃;氢火焰离子化检测器检测口温度250℃;载气为高纯氮气;分流进样,分流比1∶1;顶空加热温度85℃,平衡时间15 min。结果:二氯甲烷、三氯甲烷、三氯乙烯和二氧六环4种溶剂检测质量浓度范围内线性范围为0.002⁰.5 mg/ml(r=0.997 10.5 mg/ml(r=0.997 1⁰.999 9),苯为0.000 20.999 9),苯为0.000 2⁰.05 mg/ml(r=0.999 3)。5种有机溶剂平均加样回收率为89.1%0.05 mg/ml(r=0.999 3)。5种有机溶剂平均加样回收率为89.1%⁹3.4%,RSD为1.91%93.4%,RSD为1.91%².89%(n=3);检测限为0.012.89%(n=3);检测限为0.01⁰.3μg/ml,定量限为0.030.3μg/ml,定量限为0.03².0μg/ml。结论:本法简便、灵敏、快速、准确,适用于腺嘌呤原料药中有机溶剂残留量的测定。

Determination of 5 Residual Solvents in Adenine Raw Materials by Head-space Capillary Gas Chromatography

OBJECTIVE： To establish a method for the determination of 5 residual solvents as dichloromethane, trichlorometh- ane, benzene, trichloroethylene and dioxane in adenine raw materials. METHODS： Head-space capillary gas chromatography was adopted. Sample was prepared by 1 mol/L sodium hydroxide solution. DB-624 quartz capillary column was adopted by temperature programming; injector temperature was set at 200 ℃. FID detector was adopted with temperature of 250℃ using high purity nitro- gen as carrier gas; split sampling was adopted with splitting-ratio of 1 ： 1. The headspace vials were balanced at 85 ~C for 15 min. RESULTS： The linear ranges were 0.002-0.5 mg/ml for dichloromethane, trichloromethane, trichloroethylene and dioxane （r= 0.997 1-0.999 9） and 0.000 2-0.05 mg/ml for benzene （r----0.999 3）. Average recoveries of 5 solvents were 89.1%-93.4% （RSD=1.91%-2.89%, n=3）. The LODs and LOQs were 0.01-0.3 pg/ml and 0.03-2.0 μg/ml, respectively. CONCLUSIONS： The method is simple, sensitive, quick and accurate. It can be used for the detection of residual solvents in adenine raw materials. KEYWORDS Adenine raw materials; Head-space capillary GC; Organic solvent; Residual determination