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. 00 μm） 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.
出处
《广州化工》
CAS
2015年第23期166-167,188,共3页
GuangZhou Chemical Industry
关键词
气相色谱法
氟伐他汀钠
毛细管柱
残留溶剂
gas chromatography
fluvastatin sodium
capillary column
residual solvent
