气相色谱法测定微量乙酸乙酯含量方法研究

Amethod for the Determination of Trace Amounts of Ethyl Acetate by Gas Chromatography

目的:建立直接进样气相色谱法测定微量乙酸乙酯含量的分析方法。方法:通过对仪器参数进行优化,包括进样口温度、初始柱温、柱流速、分流比,确定最佳分析条件:色谱柱SH-PolarWax(30 m×0.32 mm 0.25μm),程序升温:初始温度为45℃,保持4min,以10℃/min升温至90℃,再以20℃/min升温至200℃;进样口温度220℃,分流比10∶1,流速1.00 m L/min。结果:在优化的色谱条件下,微量乙酸乙酯测试方法在0.01~1.00μg/mL范围内线性良好,相关系数(r)大于0.999,回收率在90%~110%范围内,RSD(n=3)均小于5%,检出限为0.004μg/mL,定量限为0.012μg/mL。结论:该方法具有检测时间短、灵敏度高的特点,研究结果可为乙酸乙酯含量检测方法研究提供数据支撑和参考。

Objective:To establish an analytical method for the determination of trace amounts of ethyl acetate by direct injection gas chromatography.Methods:The optimal analytical conditions were determined by optimizing the instrument parameters,including inlet temperature,initial column temperature,column flow rate,and split ratio:column SH-PolarWax(30 m×0.32 mm 0.25μm),programmed ramp-up:initial temperature of 45℃,hold for 4min,ramp-up to 90℃at 10℃/min,then ramp-up to 200℃at 20℃/min;inlet temperature of 220℃,flow rate of 1.00 mL/min,shunt ratio of 10∶1.Results:Under the optimized chromatographic conditions,the test method for the determination of trace amounts of ethyl acetate showed good linearity in the range of 0.01~1.00μg/mL with correlation coefficients(r)greater than 0.999,recoveries in the range of 90%~110%,RSDs(n=3)all less than 5%,detection limits of 0.004μg/mL and quantification limits of 0.012μg/mL.Conclusions:The method has the characteristics of short detection time and high sensitivity,and the research results can provide data support and reference for the research of ethyl acetate content detection method.