顶空气相色谱法测定奥拉米特中4种有机溶剂的残留量

Determination of four kinds of residual solvents in Orazamide by Headspace gas chromatography

目的采用顶空气相色谱法测定奥拉米特中4种有机溶剂的残留量。方法采用Agilent DB-624色谱柱(30 m×0.32 mm,1.8μm),经程序升温,以氮气为载气,检测器为氢火焰离子化检测器,采用顶空进样方式,用标准加入法对奥拉米特中4种有机溶剂进行定量。结果甲醇、乙酸乙酯、三氯乙烯及二甲苯在考察范围内的线性关系良好(r=0.9999),检测限分别为0.2296、0.2985、0.4956、0.2401μg·m L^-1。结论所用方法专属、灵敏、准确度高,可用于奥拉米特中溶剂残留量的测定。

OBJECTIVE To determine four kinds of residual solvents in Orazamide by Headspace gas chromatography.METHODS Chromatographic condition adopted was DB-624 capillary column(30 m×0.32 mm,1.8μm)with nitrogen as carrier gas and FID as detector.Temperature program and headspace sampling method were used.Standard addition method was used for quantitative analysis.RESULTS There was a good linear relationship between the peak area and the concentration of methanol,ethyl acetate,trichlorethylene and xylene(r=0.9999).The limit of detection were 0.2296,0.2985,0.4956 and0.2401μg·m L^-1 for methanol,ethyl acetate,trichlorethylene and xylene,respectively.CONCLUSION The method is specific,sensitive and accurate for the determination of residual solvents in Orazamide.