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
樊美霞 1汪毅 1戴鹏 1陈书蓉 1占真雄1
作者信息
- 1. 江西三鑫医疗科技股份有限公司,江西 南昌 330200
- 折叠
摘要
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 0.25 μm),程序升温:初始温度为45℃,保持4 min,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 mL/min.结果:在优化的色谱条件下,微量乙酸乙酯测试方法在 0.01～1.00 μg/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0.004 μg/mL,定量限为0.012 μg/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.
Abstract
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 0.25 μm),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 0.01～1.00 μg/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 0.004 μg/mL and quantification limits of 0.012 μg/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.
关键词
乙酸乙酯/气相色谱/条件优化/直接进样/外标法Key words
ethyl acetate/gas chromatography/condition optimization/direct injection/external standard method引用本文复制引用
出版年
2024
NETL
NSTL
万方数据