多壁碳纳米管固相萃取-气相色谱法检测蔬菜中毒死蜱、丙溴磷和三唑磷农药残留

李杨梅; 杨敏; 谭伟; 杨宏兴; 高斯祺; 李桂镇; 王红斌

doi:10.13386/j.issn1002-0306.2014.19.060

多壁碳纳米管固相萃取-气相色谱法检测蔬菜中毒死蜱、丙溴磷和三唑磷农药残留

Determination of chlorpyrifos, triazophos and profenofos in vegetables by gas chromatography with solid phase extraction using multiwalled carbon nanotubes as adsorbent

摘要

摘要: 本文以多壁碳纳米管为固相萃取材料,建立了蔬菜中毒死蜱、丙溴磷和三唑磷农药残留的GC-FPD分析方法。样品经乙酸乙酯匀浆提取后,用多壁碳纳米管SPE柱净化,以丙酮∶正己烷（1∶1,v/v）为洗脱剂,浓缩后用丙酮定容,再用GC-FPD进行检测。三种有机磷农药在0.0025².0mg/L范围内呈良好的线性关系,相关系数在0.9998⁰.9999之间,回收率在83.3%⁹6.7%之间,方法的检出限在8.21×10-4¹.37×10-3mg/kg之间。将该方法推广到莴苣、番茄、豇豆、梨、香菇等9种蔬菜、水果和食用菌中毒死蜱、丙溴磷、三唑磷农药残留的测定,效果较好。

Abstract: A method based on multiwalled carbon nanotubes as the solid phase extraction material had been developed for the determination of chlorpyrifos, triazophos and profenofos in vegetables by gas chromatographyflame photometric detector ( GC /FPD) .The samples were extracted with ethyl acetate and purified by multiwalled carbon nanotubes column.The eluent was a mixture of acetone∶hexane ( 1∶1, v /v) .Then concentrated and dissolved by acetone before determined by GC /FPD.The results showed that these pesticides had a good linearity in the range of 0.0025~2.0mg /L and the correlations were between 0.9998 and 0.9999.The recoveries rate and limits of detection were 83.3% ~ 96.7% and 8.21 × 10- 4~ 1.37 × 10- 3mg /kg. Application of the method to the analysis of chlorpyrifos, triazophos and profenofos in several samples, we had a satisfactory result.