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目的:建立乌拉地尔原料药中5种溶剂残留量的毛细管气相色谱测定方法。方法:采用Agilent DB-5毛细管气相色谱柱(30m×320μm×0.25μm),FID检测器,进样口温度200℃,检测器温度230℃;载气为高纯氮气,流速3.0mL.min-1,柱温为程序升温:40℃保持10min,10℃.min-1升温至220℃,保持5min。顶空进样,顶空瓶平衡温度80℃,平衡时间30min。结果:在上述条件下,5种残留溶剂色谱峰的理论板数均大于10 000,相邻峰的分离度均大于2;甲醇、乙醇、丙酮、二氯甲烷、1,2-二氯乙烷的线性关系良好(r分别为0.999 2,0.999 3,0.999 9,0.999 8和0.999 8);最低检出浓度分别为:0.46,0.46,0.23,0.31,0.090μg.mL-1;平均回收率均在90%以上。结论:本方法简单、准确,灵敏度高、重复性好,适用于乌拉地尔原料药中有机溶剂残留量的测定。
OBJECTIVE: To establish a method for the determination of five kinds of residual solvents in Urapidil by capillary gas chromatography. Methods: Agilent DB-5 capillary gas chromatography column (30m × 320μm × 0.25μm) and FID detector were used. The inlet temperature was 200 ℃ and the detector temperature was 230 ℃. The carrier gas was high purity nitrogen and the flow rate was 3.0mL · min- 1, column temperature for the program temperature: 40 ℃ for 10min, 10 ℃. Min-1 temperature to 220 ℃, hold 5min. Headspace injection, headspace bottle balance temperature 80 ℃, balance time 30min. Results: Under these conditions, the number of theoretical plates of the five residual solvent peaks were more than 10 000 and the resolution of adjacent peaks were both greater than 2. The separation of methanol, ethanol, acetone, methylene chloride, 1,2-dichloroethane (R = 0.999,0.999 3,0.999 9,0.999 8 and 0.999 8, respectively). The minimum detectable concentrations were 0.46,0.46,0.23,0.31,0.090μg.mL-1 respectively. The average recovery was More than 90%. Conclusion: The method is simple, accurate, sensitive and reproducible. It is suitable for the determination of residual organic solvents in Urapidil.