毛细管气相色谱法测定伏立康唑中6种有机溶剂残留量

Capillary GC determination of 6 residual organic solvents in voriconazole

目的:建立伏立康唑中6种有机溶剂残留量的测定方法。方法:使用配置顶空进样器的毛细管气相色谱仪,采用 DB-624毛细管色谱柱(94%二甲基聚硅氧烷和6%氰丙基苯聚硅氧烷),0.53 mm×30 m,液膜厚度为3μm;柱温50℃,保持10min,以10℃·min^(-1)的速度升温至100℃;以氮气为载气,流速为2 mL·min^(-1);FID 检测器。结果:甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯和四氢呋喃线性关系良好,相关系数均大于0.999;平均回收率分别为97.9%,102.8%,95.8%,106.3%,104.5%,101.2%;检出限分别为1.6,1.5,4.7,1.2,1.7,1.7μg·mL^(-1)。结论:本方法简便,灵敏度高,重复性好,结果准确,适合于伏立康唑中有机溶剂残留量的测定。

Objective：To establish a CGC method for determination of six residual organic solvents in voriconazole. Methods：The CGC was equipped with a headspace injector and a flame -ionization detector. A 0. 53 mm × 30 m DB -624 capillary chromatographic column（ coated with 94% dimethylpolysiloxane and 6% cyanopropyl -polysiloxane stationary phase） was adopted and the carrier gas was nitrogen. The initial column temperature was kept at 50 ℃ for 10 min,then raised to 100 ℃ at the rate of 10 ℃ · min^-1. Result：The correlation coefficient in methanol, acetone, isopropanol, dichloromethane, ethyl acetate and tetrahydrofuran were all higher than 0. 999. The recovery were 97.9%, 102. 8% ,95.8%, 106.3%, 104. 5%, 101.2% and limit of detection respectively were 1.6,1.5, 4.7,1.2,1.7,1.7 μg · mL^- 1. Conclusion： This method appeared to be sensitive, accurate, repeatable and easy to operate.