卡马西平中残留溶剂的研究

Study of Residual Solvents in Carbamazipine

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 & method for determining residual solvents such as chlorobenzene,methanol and ethanol in Carbamazipine by headspace gas chromatography.Methods:The GC was equiped with a headspace injector and a flame-ioniza-tion detector. A HP-INNMWAX(Crosslinked polyethylene glycol) ,30m×0. 32mm×0. 25μm was adopted. The carrier gas was nitrogen. The assay of residual solvents were calculated according to the external standard method. Results:Methanol and ethanol were found in the sample of Carbamazipine. The standard curves were liner over the range of 0. 07-3. 62μg·ml-1(r = 0. 9992) for chlorobenzene,0. 60-30. 1μg·ml-1(r = 0. 9978) for methanol and 1. 00-50.08μg·ml-1(r = 0. 9986) for ethanol, respectively. The limits of quantitation were 0.1μg ·ml-1 for chlorobenzene, 0. 7μg·ml-1 for methanol and 0. 4μg ·ml-1 for ethanol,respectively. The average recoveries were 99. 12%(RSD = 2. 52%,n = 6) for chlorobenzene,97. 51%(RSD=4. 31%,n = 6) for methanol and 98. 52%(RSD=3.12%,n = 6) for ethanol. Conclusion:This method appeared to be sensitively accurate,repeatable and easy to operate.