顶空气相色谱法测定氟伐他汀钠中5种残留溶剂

摘要

建立氟伐他汀钠中5种残留溶剂（甲醇、丙酮、正己烷、乙酸乙酯、四氢呋喃）的测定方法。采用毛细管顶空气相色谱法， DB－624毛细管色谱柱（30 m×0.530 mm 3.00μm）， FID检测器，载气为氮气，程序升温，柱温为50℃，维持8 min，以20℃／min升温至200℃，维持3 min，进样口温度为200℃，检测器温度为250℃，分流进样模式，用正丙醇作为内标物，按内标法计算残留溶剂的结果。结果表明：各成分在考察的浓度范围内具有良好的线性关系（5种成分的相关系数均为0.999以上），5种成分3个浓度的回收率均在90.0％～110.0％之间。精密度RSD均＜1.0％。结论所建方法专属性强，灵敏度好，操作简便，结果可靠，可用于氟伐他汀钠中5种残留溶剂的同时测定。%To establish a method for determination of five residual solvents ( Methanol, Acetone, n-Hexane, Ethyl Acetate, Tetrahydrofuran) in Fluvastatin Sodium, Capillary Headspace Gas Chromatography was used for determination of residue solvents.DB-624 capillary column (30 m×0.530 mm, 3.00μm) was used with FID as detector and nitrogen as carrier gas.The column temperature was programmed from 50 ℃ ( 8 min ) to 200 ℃ ( 3 min ) at 20 ℃/min.The injector temperature was 200℃, and the detector temperature was 250℃, with split-inject mode.The internal standard was n-propanol and the amount of residul solvents can be calculated through internal standard method.Good linearity was obtained in the experimental concentration range ( r>0.999 ) .The recoveries were in the range of 90.0 ~110.0.The RSDs were all less than 1.0%.The method is specific, sensitive, simple and credible which can be used for determination of five residual solvents in fluvastatin sodium at the same time.