毛细管气相色谱法测定巴胺磷溶液含量

Determination of Propetamphos in Propetamphos Solution by Capillary Gas Chromatography

建立了毛细管气相色谱法测定巴胺磷溶液含量的方法。试验采用6%氰丙基苯基-94%二甲基硅氧烷为固定相的毛细管柱,柱温240℃,进样口温度250℃,FID检测器温度250℃,载气为氮气,流速3 mL/min,进样量1μL,分流比15∶1,内标物质为邻苯二甲酸二丁酯。在该色谱条件下,巴胺磷峰与内标物质峰分离度良好,方法平均回收率为103.5%(n=9,RSD=1.7%),重复性RSD为0.6%,定量限为2.5μg/mL,巴胺磷在0.025~0.5 mg/mL浓度范围内呈良好的线性关系(r^(2)=0.9999),不同色谱柱、柱温、流速、进样口温度、检测器温度耐用性良好。结果表明,建立的方法专属性好、快速、准确,可用于测定巴胺磷溶液的含量。

A method for determination of propetamphos in propetamphos solution by capillary gas chromatography was developed.The capillary column with 6%cyanopropyl phenyl-94%dimethyl polysiloxane as stationary phase was used.The column temperature was 240℃,the inlet temperature was 250℃,FID was used as detector and the temperature was 250℃,the carrier gas was nitrogen,the flow rate was 3 mL/min,the injection volume was 1μL,the split ratio was 15∶1,and the internal standard material was dibutyl phthalate.In this chromatographic condition,a good separation was accepted between propetamphos and the internal standard material.The average recovery of the method was 103.5%,and the RSD was 1.7%(n=9).The RSD of repeatability was 0.6%.The limit of quantitation was 2.5μg/mL.Propetamphos showed good linear relationship within the range of 0.025~0.5 mg/mL(r^(2)=0.9999).The robustness of different column,oven temperature,flow rate,inlet temperature and detector temperature was good.In conclusion,this method is specific,rapid and accurate for the determination of propetamphos in propetamphos solution.