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目的:建立美罗培南原料药中丙酮、乙睛、二氯甲烷、四氢呋喃和乙酸乙酯有机溶剂残留量的顶空气相色谱测定法。方法:色谱条件:FID检测器,DB-624石英毛细管柱(30 m×0.321 mm×1.80μm),柱温50℃。结果:丙酮、乙睛、二氯甲烷、四氢呋喃、乙酸乙酯分别在0.025～139.600、0.053～70.700、0.012～39.800、0.016～70.100、0.039～43.000 mg·ml~(-1)的浓度范围内线性关系良好(r>0.999 0);丙酮、乙睛、二氯甲烷、四氢呋喃、乙酸乙酯的回收率分别为:97.7%、96.7%、98.3%、95.4%、96.6%,RSD均小于5.0%。结论:本方法简便、准确、重复性好,可在同一色谱系统中测定美罗培南原料生产过程中残留的5种有机溶剂。
OBJECTIVE: To establish a headspace gas chromatographic method for the determination of the residual organic solvents in Meropenem APIs such as acetone, ethyl acetate, methylene chloride, tetrahydrofuran and ethyl acetate. Methods: Chromatographic conditions: FID detector, DB-624 quartz capillary column (30 m × 0.321 mm × 1.80 μm) with a column temperature of 50 ℃. Results: Acetone, acetonitrile, methylene chloride, tetrahydrofuran and ethyl acetate were linear in the range of 0.025 ~ 139.600,0.053 ~ 70.700,0.012 ~ 39.800,0.016 ~ 70.100,0.039 ~ 43.000 mg · ml ~ (-1) (R> 0.999 0). The recoveries of acetone, acetonitrile, methylene chloride, tetrahydrofuran and ethyl acetate were 97.7%, 96.7%, 98.3%, 95.4% and 96.6%, respectively. The RSDs were less than 5.0%. Conclusion: The method is simple, accurate and reproducible. Five organic solvents remaining in the raw materials of Meropenem can be determined in the same chromatographic system.