顶空气相色谱法测定氯苯达诺原料药中的残留溶剂含量

Determination of Residual Solvent in Clofedanol by Gas Chromatography with Headspace Sampling

摘要: 目的：建立顶空气相色谱法检验氯苯达诺盐酸盐原料药中残留溶剂的方法。方法：采用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱(DB-624, 0.53 mm × 30 m, 3.0 μm)，程序升温，初始温度40℃，保持3 min，以20℃/min的速率升温至240℃，保持3 min；氢火焰离子化检测器(FID)，检测器温度250℃，进样口温度200℃，载气为氦气，流速5 mL/min，进样体积1 mL。分流比1:1。结果：5种有机溶剂(甲醇、乙醇、乙腈、苯、甲苯)进样浓度与峰面积呈良好线性关系，相关系数均大于0.9990，加样回收率在96.0%~103.0%之间。结论：此法准确可靠，灵敏度高，可用于氯苯达诺中残留溶剂的测定。

Abstract: Objective: To establish a GC method for the determination of residual solvent in clofedanol. Methods: DB-624 chromatographic column (coated with 6% cyanopropylphenyl-94% dimethylpolysiloxane, length 30 m, I.D. 0.53 mm, film 3.0 μm) was adopted. The column temperature was programmed, kept at 40˚C for 3 min, and then increased by 20˚C/min to 240˚C for 3 min. The temperature of FID detector was 250˚C and the temperature of inlet was 200˚C. The carrier gas was He at a flow rate of 5 mL/min. The injection volume was 1 mL. Results: The calibration curves of five solvents all showed good linearity in a detected concentration range (r > 0.9990); the range of average recovery was between 96.0% and 103.0%. Conclusion: The method was accurate, reliable and sensitive, and can be used for assay of residual organic solvent in clofedanol.