QuEChERS-HPLC-MS/MS法快速筛查与确证人参花中14种农药残留

建立了QuEChERS-高效液相色谱-三重四极杆质谱法测定人参花中14种农药残留的分析方法。样品使用1%醋酸乙腈进行初步提取,再用乙二胺-N-丙基硅烷(PSA)、C18和石墨化炭黑(GCB)这3种吸附剂进行净化,采用多反应监测模式(MRM)进行检测,基质外标法定量。结果表明,14种农药的浓度和样品峰面积在0.5~100μg/L范围内呈良好线性关系(R²>0.999),在3个添加水平下测得回收率在70.8%~108.7%之间,测定结果的相对标准偏差在2.06%~10.35%范围内(n=6)。该方法灵敏度高、净化效果好,可同时快速检测人参花中多种农药残留,具有良好的定性和定量检测性能。

QuEChERS-HPLC-MS/MS Method for Rapid Screening and Confirmation of 14 Pesticide Residues in Ginseng Flowers

A method based on QuEChERS-high-performance liquid chromatography triple quadrupole mass spectrometry(HPLC-MS/MS)was established for the determination of 14 pesticide residues in ginseng flower.The samples were initially extracted with 1%acetonitrile acetate.The extract was purified with ethylenediamine-N-propyl silane(PSA),C18 and graphitized carbon black(GCB).After that,the samples were detected by multiple reaction monitoring mode(MRM)and quantified by matrix external standard method.The analytical results showed that the calibration curves for the 14 pesticides obtained by HPLC-MS/MS were linear in the range of 0.5~100μg/L,with the correlation coefficients higher than 0.999.The recoveries ranged from 70.8%to 108.7%with relative standard deviations(RSDs)ranging from 2.06%to 10.35%at the three supplemental levels(n=6).This method has the advantages of high sensitivity and good purification effect.The proposed method can simultaneously detect multi-pesticides residues with a good performance in terms of qualitative and quantitative detection.