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目的:建立顶空气相色谱法测定西咪替丁原料药中环己烷、丙酮、甲醇、乙醇4种溶剂残留量的方法。方法:色谱柱为键合聚乙二醇毛细管柱;载气为氮气,程序升温;进样口温度为150℃,检测器温度为220℃;分流比为1∶1;流速为5.0mL·min-1;顶空进样,以外标法计算残留溶剂含量。结果:环己烷、丙酮、甲醇、乙醇的检测浓度线性范围分别为0.1488~2.381、0.1826~3.287、0.1496~2.693、0.1448~2.317mg·mL-1,最低检测限分别为0.05~1.2μg;平均回收率在99%以上(RSD≤1.0%,n=5)。结论:该方法灵敏、可靠,重复性好,结果准确,可用于西咪替丁原料药中有机溶剂残留量的测定。
OBJECTIVE: To establish a method for the determination of 4 solvents residues of cimetidine, cetomacrogol, methanol and ethanol by headspace gas chromatography. Methods: The column was a bonded polyethylene glycol capillary column. The carrier gas was nitrogen and the temperature was programmed. The inlet temperature was 150 ℃, the detector temperature was 220 ℃, the split ratio was 1: 1, the flow rate was 5.0mL · min -1; headspace sampling, calculated by external standard residual solvent content. Results: The linear range of detection concentration of cyclohexane, acetone, methanol and ethanol were 0.1488 ~ 2.381,0.1826 ~ 3.287,0.1496 ~ 2.693,0.1448 ~ 2.317mg · mL-1, respectively. The detection limits were 0.05 ~ 1.2μg, The recovery was above 99% (RSD ≤ 1.0%, n = 5). Conclusion: The method is sensitive, reliable, reproducible and accurate. It can be used for the determination of organic solvent residues in cimetidine raw materials.