气相色谱法测定9种拟除虫菊酯类农药的研究

Study on the method for determination of 9 kinds of pyrethroids pesticide by gas chromatography

目的建立一种气相色谱法同时测定9种拟除虫菊酯类农药的检测方法。方法通过选择色谱柱,优化仪器参数,得出9种目标物分离的最佳检测条件。结果色谱柱选择弱极性色谱柱(0.25 mm×30 m,0.25μm);仪器参数设定为间歇不分流-程序升温;色谱柱升温程序:初始温度100℃,保持0.75 min,以30℃/min升至220℃,再以2℃/min升至250℃,然后以25℃/min升至280℃,保持5 min,最后以10℃/min升至300℃,保持7 min;载气流速:2.0 ml/min;进样口温度:260℃;检测器的温度:310℃。在该条件下9种目标物取得很好的分离效果,定量分析呈现良好的线性关系,相关系数>0.99。结论该方法仪器配置要求低,易于推广,对于有关部门检测拟除虫菊酯类农药残留具有借鉴意义。

Objective To establish a kind of detection method for simultaneous determination of 9 kinds of pyrethroids pesticide by gas chromatography,so as to provide technical reference for the relevant quality inspection department to inspect the pyrethroid pesticide residues in agricultural products,aquatic products,medicine,water and air. Methods By selecting the chromatographic column,and optimizing the instrument parameters,the optimum testing conditions of 9 kinds of target separation was acquired. Results The weak polarity column（0. 25 mm × 30 m,0. 25 μm） was chose as the chromatographic column.The instrument parameters were setted at intermittent splitless-temperature programmed. The chromatography column temperature program were following： initial temperature was 100 ℃,keeping 0. 75 min,raised to 220 ℃ by 30 ℃ / min,and to 250 ℃by 2 ℃ / min,and then raised by 25 ℃ / min to 280 ℃ to keep 5 min,finally up to 300 ℃ with 10 ℃ / min,keeping 7 min. The carrier gas flow rate was 2. 0 ml / min; Injection temperature was 260 ℃; Detector temperature was 310 ℃. Under the condition,the nine target achieved good separation effect,and the quantitative analysis had good linear relationship with correlation coefficients were greater than 0. 99. Conclusion The method was low of instrument configuration requirements and easy to promote,and had a reference significance for related departments to study method for detecting pyrethroids pesticide residues.