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

关键词:  毛细管气相色谱法  巴胺磷溶液  含量测定

Key words:  capillary gas chromatography  propetamphos solution  determination of content

摘要:

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1 μL,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2.5 μg/mL,巴胺磷在0.025~0.5 mg/mL浓度范围内呈良好的线性关系(r²=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。

Abstract:

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 1 μL, 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 2.5 μg/mL. Propetamphos showed good linear relationship within the range of 0.025~0.5 mg/mL (r²=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.