通过型固相萃取-液相色谱-高分辨质谱法快速测定粮谷中17种酰胺类农药残留量

应用PRiME HLB固相萃取柱通过式净化技术,采用液相色谱-四极杆静电场轨道阱高分辨质谱(LC-Q Orbitrap),建立了粮谷中17种酰胺类农药的检测方法。样品经乙腈提取,PRiME HLB固相萃取柱净化,在GL Intersil ODS-3色谱柱上以0.5%甲酸水和乙腈为流动相进行梯度洗脱,四极杆静电场轨道阱高分辨质谱以Full Scan/ddMS^2模式进行检测。结果表明,各组分在各自浓度范围内线性关系良好,相关系数均大于0.996。方法定量限在0.5~5μg/kg之间。待测物在5.0,10.0,50.0μg/kg 3个浓度水平下加标回收率在70.4%~101.6%之间,相对标准偏差在2.7%~10.8%之间。该方法可用于粮谷中酰胺类农药的测定。

Rapid determination of 17 amide pesticides residues in grains by going through column purification-liquid chromatography-high resolution mass spectrometry

A method was developed for the determination of the 17 amide pesticides residues in grains by liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry(LC-Q Orbitrap)with PRiME HLB column going through purification technique.Samples were extracted with acetonitrile,purified with a PRiME HLB column,and detected by LC-Q Orbitrap in full scan/ddMS^2 mode after gradient elution on a GL Intersil ODS-3 column with 0.5%formic acid solution and acetonitrile as mobile phase.The results showed good linear relationships for the components in their respective concentration ranges with the correlation coefficients of higher than 0.996.The limits of quantitation(LOQs)were in the range of 0.5-5μg/kg.The average recoveries at different levels(5,10 and 50μg/kg)for all the analytes ranged from 70.4%to 101.6%,with the relative standard deviations of 2.7%-10.8%.This proposed method could be applied to determine amide pesticides residues in grains.