顶空毛细管气相色谱法测定非那甾胺原料药中有机溶剂残留量  

Determination of Residual Organic Solvents in Finasteride Raw Materials by Headspace Capillary Gas Chromatography

作　　者：郭文献[1] 辜鹏程[1] 李勤耕[1] 

机构地区：[1]重庆医科大学药学院,重庆400016

出　　处：《中国药房》2013年第17期1604-1606,共3页China Pharmacy

摘　　要：目的:建立测定非那甾胺原料药中甲醇、丙酮、三氯甲烷及甲苯4种有机溶剂残留量的方法。方法:采用顶空毛细管气相色谱法。色谱柱为PhenomenexZB-624毛细管柱,二甲基亚砜为溶剂,柱温采用程序升温,进样口温度为200℃,氢火焰离子化检测器检测口温度为250℃,载气为N2,分流比为5∶1,顶空进样,平衡温度为80℃,平衡时间为45min。结果:4种有机溶剂实现基线分离,甲醇、丙酮、三氯甲烷及甲苯的线性范围分别12.0～1200、10.0～1000、1.20～120、1.78～178μg/m(lr为0.9996～0.9998);平均方法回收率为94.7%～97.5%,RSD<2.1%;检测限为0.0216～10.93μg/ml。5批样品中4种有机溶剂残留量均符合2010年版《中国药典》要求。结论:该方法灵敏、重复性好,可用于非那甾胺原料药中有机溶剂残留量的测定。OBJECTIVE： To establish the method for the determination of 4 residual organic solvents in finasteride raw materials, i.e. methanol, acetone, chloroform and methylbenzene. METHODS： Headspace gas chromatography was adopted. The residual organic solvents were separated on phenomenex ZB-624 capillary column using dimethyl sulfoxide as solvent by temperature programming. FID was used as detector with a temperature of 250 ℃. The inlet temperature was 200 ℃. N2 was used as carrier gas with split ratio of 5 ： 1. With headspace sampling, equilibrium temperature was 80 ℃ and equilibrium time was 45 min. RESULTS： The linear ranges of methanol, acetone, chloroform and methylbenzene were 12.0-1 200, 10.0-1 000, 1.20-120 and 1.78-178 μg/ ml （r=0.999 6-0.999 8）, respectively. Recovery rates were 94.7%-97.5% （RSD〈2.1%）; the detection limits were in the rang of 0.021 6 to 10.93 μg/ml. Residual amount of 4 organic solvents in 5 batches of samples were in line with the requirements of Chinese Pharmacopeia （2010 edition）. CONCLUSIONS： The method is sensitive and reproducible. It can be applied for the determination of the residual organic solvents in finasteride raw materials.

关 键 词：顶空毛细管气相色谱法 非那甾胺 原料药 有机溶剂 残留量 

分 类 号：R927.2[医药卫生—药学] R983