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建立了顶空毛细管色谱法测定加巴喷丁原料药中4种三类残留溶剂的方法。采用气相色谱顶空进样法,以水:DMF(9:1,V/V)为溶剂,DB-624为分析柱,采用程序升温:初始柱温35℃保持3 min,以10℃/min的升温速率升至155℃,保持4 min,再以30℃/min的升温速率升至245℃,保持5 min。结果表明:4种残留溶剂色谱峰面积与浓度线性关系良好,加标回收率结果满意。本方法可用于加巴喷丁原料药中残留溶剂乙醇、丙酮、异丙醇和三乙胺的检测。
A method for the determination of four kinds of three types of residual solvents in gabapentin raw material by headspace capillary chromatography was established. The GC-headspace sampling method was used. The temperature was set at 35 ℃ for 3 min and the temperature was increased by 10 ℃ / min with DMF: 9: 1, V / V as solvent and DB-624 as analytical column. The heating rate was raised to 155 ° C for 4 min and then to 245 ° C at a ramp rate of 30 ° C / min for 5 min. The results showed that the linear relationship between the chromatographic peak areas and the concentrations of the four residual solvents was good, and the recoveries of spiked samples were satisfactory. The method can be applied to the detection of residual solvents such as ethanol, acetone, isopropanol and triethylamine in gabapentin raw material.