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目的:用气相色谱的顶空进样法建立卡马西平中的残留溶剂氯苯、甲醇和乙醇的测定方法。方法:使用配置顶空进样器的气相色谱仪,采用HP-INNOWAX(交联聚乙二醇),30m×0.32mm×0.25μm色谱柱,以氦气为载气,FID检测器,顶空进样。通过外标法计算残留溶剂的含量。结果:卡马西平中有残留溶剂甲醇、乙醇检出。标准曲线的线性范围:氯苯为0.07-3.62μg·mL(r=0.9992),甲醇为0.60-30.1μg·mL-1(r=0.9978),乙醇为1.00-50.08μg·mL-1(r=0.9986),定量限氯苯为0.1μg·mL-1,甲醇为0.7μg·mL-1,乙醇为0.4μg·mL-1;平均回收率氯苯为99.12%(RSD=2.52%,n=6),甲醇为97.51%(RSD=4.31%,n=6),乙醇为98.52%(RSD=3.12%,n=6)。结论:本方法简便,灵敏度高,重复性好,结果准确。
OBJECTIVE: To establish a method for the determination of chlorobenzene, methanol and ethanol in carbamazepine by headspace gas chromatography. Methods: A gas chromatograph equipped with a headspace sampler, HP-INNOWAX (cross-linked polyethylene glycol), 30m × 0.32mm × 0.25μm column with helium as carrier gas, FID detector, Injection. Calculate residual solvent content by external standard method. Results: carbamazepine residual solvents methanol, ethanol detected. The linear range of the standard curve was 0.07-3.62 μg · mL (r = 0.9992) for chlorobenzene, 0.60-30.1 μg · mL -1 (r = 0.9978) for methanol and 1.00-50.08 μg · mL -1 for ethanol (r = 0.9986), the limit of quantification of chlorobenzene was 0.1μg · mL-1, methanol was 0.7μg · mL-1 and ethanol was 0.4μg · mL-1. The average recoveries of chlorobenzene were 99.12% (RSD = 2.52%, n = 6 ), 97.51% for methanol (RSD = 4.31%, n = 6) and 98.52% for ethanol (RSD = 3.12%, n = 6). Conclusion: The method is simple, high sensitivity, good repeatability and accurate results.