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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 a method for the determination of 4 organic solvents residues of methanol, acetone, chloroform and toluene in finasteride. Methods: Headspace capillary gas chromatography. The column was PhenomenexZB-624 capillary column, dimethyl sulfoxide as solvent, the column temperature was programmed temperature, the inlet temperature was 200 ℃, hydrogen flame ionization detector detection port temperature was 250 ℃, the carrier gas was N2, shunt Ratio of 5: 1, headspace injection, the equilibrium temperature is 80 ℃, the balance time is 45min. Results: The baseline separation of four organic solvents was achieved. The linear range of methanol, acetone, chloroform and toluene were 12.0 ~ 1200, 10.0 ~ 1000, 1.20 ~ 120 and 1.78 ~ 178μg / The recoveries ranged from 94.7% to 97.5% with a RSD <2.1%. The detection limits were 0.0216-10.93μg / ml. The remaining four organic solvents in 5 batches of samples all met the requirements of the 2010 edition of “Chinese Pharmacopoeia”. Conclusion: The method is sensitive and reproducible and can be used for the determination of residual organic solvents in finasteride.