药物资讯

Vol.4 No.3 (August 2015)

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

 

作者:

王 琳 , 丁海宏 , 张智红 , 胡 丽 :江苏宝众宝达药业有限公司,江苏 南通

 

关键词:

顶空色谱法氯苯达诺残留溶剂GC Clofedanol Residual Solvent

 

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。

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.

文章引用:

王 琳 , 丁海宏 , 张智红 , 胡 丽 (2015) 顶空气相色谱法测定氯苯达诺原料药中的残留溶剂含量。 药物资讯, 4, 31-34. doi: 10.12677/PI.2015.43004

 

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