基于UPLC-MS/MS检测番茄中10种杀虫剂农药残留

[目的]建立了同时检测番茄中10种杀虫剂残留的分析方法。[方法]采用乙腈提取番茄中的农药有效成分,并在常规QuEChERS吸附剂中添加新型吸附剂(石墨烯和碳纳米管)进行净化,采用超高效液相-质谱联用法(UPLC-MS/MS)分析,对9种吸附剂组合的净化效果进行对比研究。[结果]10种杀虫剂的检出限为1~4μg/kg,定量限为10μg/kg;添加石墨烯和碳纳米管的吸附剂组合,对色素的净化效果优于常规吸附剂,且分层效果好;番茄中10种杀虫剂的最佳净化吸附剂组合为PSA 50 mg+无水硫酸镁150 mg+碳纳米管2 mg;番茄中7种杀虫剂不存在明显的基质效应,3种杀虫剂存在明显的基质抑制效应;10种杀虫剂在番茄中3个水平的添加回收率在65.75%~110.88%范围内,符合农药残留痕量分析试验要求。[结论]证明该分析方法适用于番茄中该10种杀虫剂的痕量残留分析,且具有灵敏度高,重复性好,价格低廉等优点。

Detection of 10 Pesticides Residues in Tomato Based on UPLC-MS/MS

[Aims]An analytical method for the determination of 10 pesticide residues in tomato was established.[Methods]The effective components of pesticides in tomato were extracted with acetonitrile,and new adsorbents(graphene and carbon nanotubes)were added into the conventional QuEChERS adsorbent for purification.Ultra High Performance Liquid Chromatography-Mass Spectrometry(UPLC-MS/MS)was used for analysis,and the purification effect of 9 sorbent combinations was compared and studied.[Results]The results showed that the detection limit of 10 insecticides was 1 to 4μg/kg,and the quantitative limit was 10μg/kg.Adding the adsorbent combination of graphene and carbon nanotubes,the purification effect of pigment is better than that of conventional adsorbent.The best purification adsorbent combination of 10 insecticides in tomato was PSA 50 mg+150 mg anhydrous magnesium sulfate+2 mg carbon nanotubes.In tomato,7 insecticides had no obvious matrix effect and 3 insecticides had obvious matrix inhibition effect.The addition recovery at 3 levels of 10 insecticides in tomato ranged from 65.75 to 110.88%,which met the requirements of trace pesticide residue analysis test.[Conclusions]In summary,it is proved that the analytical method is suitable for the trace residue analysis of 10 insecticides in tomato,it has the advantages of high sensitivity,good repeatability and low price.