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目的用毛细管柱气相色谱法建立盐酸伊立替康中残留溶剂(甲醇、无水乙醇、丙酮、三氯甲烷、吡啶)的测定方法。方法采用DB-5(0.53mm×30m,5.00μm)毛细管柱(固定相为5%二苯基-95%二甲基硅氧烷共聚物),以氮气为载气,FID检测器,采用程序升温,分流直接进样,外标法计算残留溶剂的含量。结果在考察的浓度范围内呈现良好的线性关系(甲醇r=0.9997,无水乙醇r=0.9997,丙酮r=0.9997,三氯甲烷r=0.9995,吡啶r=0.9998),平均回收率范围为97.3%～101.1%,理论塔板数均>5000,相邻的溶剂峰的分离度均>2,精密度RSD<3%。结论本方法简单、结果准确、重现性好,可用于盐酸伊立替康中甲醇、无水乙醇、丙酮、三氯甲烷、吡啶5种残留溶剂的同时测定。
Objective To establish a method for the determination of residual solvents (methanol, absolute ethanol, acetone, chloroform, pyridine) in irinotecan hydrochloride by capillary gas chromatography. Methods The capillary column with DB-5 (0.53mm × 30μm, 5.00μm) was used as stationary phase (5% diphenyl-95% dimethylsiloxane copolymer) with nitrogen as carrier gas and FID detector. Heating, shunt direct injection, external standard method to calculate the residual solvent content. The results showed a good linear relationship (r = 0.9997 for methanol, r = 0.9997 for ethanol, r = 0.9997 for acetone, r = 0.9995 for chloroform and 0.9998 for pyridine) with the average recoveries ranged from 97.3% ~ 101.1%, the number of theoretical plates were more than 5000, the resolution of adjacent solvent peaks were both> 2, and the RSD of precision was <3%. Conclusion The method is simple, accurate and reproducible. It can be used for the simultaneous determination of five residual solvents, ie, methanol, ethanol, acetone, chloroform and pyridine in irinotecan hydrochloride.