毛细管气相色谱法检测普伐他汀中有机溶剂的残留量

目的:建立以毛细管气相色谱法检测普伐他汀原料药中有机溶剂残留量的方法。方法:检测器为氢火焰离子化检测器(FID),色谱柱为DB-5毛细管色谱柱,初始柱温为40℃,保持3min后以40℃.min-1升至180℃,保持3min,进样口温度为200℃,检测器温度为240℃,进样量为0.3μL,检测对象为9种溶剂,包括甲醇、乙腈、二氯甲烷、正己烷、三氯甲烷、四氢呋喃、乙酸乙酯、甲苯、N,N-二甲基甲酰胺。结果:9种有机溶剂实现基线分离,线性关系良好(r均大于0.998 9),平均回收率为98.5%～100.8%,RSD=2.0%～4.2%,最低检测浓度为0.10～1.38ng.mL-1,均未在普伐他汀原料药中检出。结论:本方法操作简便、结果准确,可用于普伐他汀原料药中有机溶剂残留量的测定。

Determination of Residual Levels of Organic Solvents in Pravastatin by Capillary Gas Chromatography

OBJECTIVE： To apply capillary gas chromatography （GC） to determine the residual levels of organic volatile solvents in pravastatin. METHODS： Flame ionization detector was used. GC determination of sample was carried out on DB- 5 sillica capillary column at an initial temperature of 40℃ for 3 min followed by an increase at the rate of 40·min^-1 to 180℃, which was maintained for 3 min. The injection port temperature was kept at 200℃ and detector temperature was kept at 240℃. The injection volume was 0.3μL. The 9 kinds of solvents includes （methanol, acetonitrile, dichloromethane, N-hexane, chloroform, tetrahydrofuran, ethyl acetate, toluene, N,N-dimethylformamide）. RESULTS： Baseline separation of 9 organic sol-vents achieved. All had good linear relationship （r 〉 0.998 9 for all solvents）, with their average recovery rates stood at 98.5%～100.8% （RSD = 2.0%～4.2%） . The minimum detectable concentration was 0.10～1.38 ng·mL^-1, all of solvents can＇t be detected out in raw material of pravastatin. CONCLUSION： This method is simple in operation and rapid in results, and it is suitable for the determination of the residual levels of organic volatile solvents in raw material of pravastatin.