顶空毛细管气相色谱法测定酚磺乙胺中乙醇及1,2-二氯乙烷残留量

Determination of Residual 1,2-Dichloroethane and Ethanol in Etamsylate Materials by Head-space Capillary GC

目的:建立顶空毛细管气相色谱法测定酚磺乙胺中的乙醇及1,2-二氯乙烷残留量分析方法。方法:采用外标法,DB-624毛细管色谱柱(30 m×0.32 mm,1.80μm),火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。柱程序升温:起始温度40℃,保持6 min,再以10℃·min^(-1)的速率升温至60℃,保持5 min,再以10℃·min^(-1)的速率升温至150℃,保持2 min。载气为氮气;流速为1.0 ml·min^(-1);分流进样,分流比为5:1。顶空条件:平衡温度65℃,平衡时间为30 min,进样量:1ml。结果:各组分完全分离,线性关系良好(R^2>0.998 0),平均回收率分别为98.84%(RSD=1.79%)和98.92%(RSD=1.26%)。结论:本法简便、准确、精确,适用于酚磺乙胺原料中乙醇和1,2-二氯乙烷残留量的同时检测。

Objective：To establish a head-space capillary GC method for the determination of residual ethanol and 1,2-dichloroethane in etamsylate materials.Method：An external standard method was used.The analytical column was a DB-624 capillary column（30 m×0.32 mm,1.80 μm） with an FID detector.The injector temperature was 2001 and the detector temperature was 250℃.The initial temperature was 40℃（kept for 6 min）,then risen to 60℃ at a rate of 10℃？min-1（kept for 5 min）,and finally risen to 150℃ at the rate of 10℃？min-1（kept for 2 min）.Result：All the solvents could be completely separated with good linear relationship（R2 ＆gt; 0.998 0）.The average recovery of ethanol and 1,2-dichloroethane was respectively 98.84%（RSI） = 1.79%） and 98.92%（RSD = 1.26%）.Conclusion：The method is simple,accurate,sensitive and repealable,and can be used in the determination of residual solvents in etamsylate.