QuEChERS-高效液相色谱/串联质谱法同时测定蜂蜜中9种新烟碱类杀虫剂残留

Determination of Nine Neonicotinoid Insecticides in Honey by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了蜂蜜中吡呀酮、吡虫啉、啶虫脒、噻虫嗪、噻虫啉、烯啶虫胺、噻虫胺、呋虫胺和氯噻啉9种新烟碱类杀虫剂的QuEChERS-高效液相色谱/串联质谱（HPLC-MS/MS）检测方法。样品以水提取,采用N-丙基乙二胺（PSA）和酸性Al2O3净化,用Zorbax Eclipse Plus C18柱（100×3.0mm,1.8μm）分离,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,采用电喷雾正离子模式（ESI^＋）、多重反应监测（MRM）检测目标分析物,基质匹配标准溶液外标法定量。结果表明：9种杀虫剂均具有良好的线性关系（r^2〉0.9969）;方法检出限为0.3-0.8μg/kg;定量限为1.0-2.5μg/kg;在2.5、10、25μg/kg三个添加水平下,杂花蜜、油菜蜜、棉花蜜和葵花蜜四种基质样品中9种杀虫剂的平均回收率在81.7%-106.7%范围,相对标准偏差（RSDs）在4.2%-9.4%之间。该方法分析速度快、灵敏度高、重现性好,适用于蜂蜜中新烟碱类杀虫剂残留的快速检测和确证。

A method was developed for the determination of nine neonicotinoid insecticides in honey by using QuEChERS-high performance liquid chromatography coupled with tandem mass spectrometry（HPLC-MS/MS）.The samples were extracted with water,and then cleaned up by N-n-propylethylenediamine（PSA）and acidic Al2O3.The analytes were separated on a Zorbax Eclipse Plus C18column（3.0×100mm,1.8μm）using acetonitrile-0.1%formic acid solution as the mobile phase in gradient elution.The analysis process was performed under electrospray positive ion source（ESI^＋）and multiple reaction monitoring mode（MRM）,and the targets were quantified by matrix-matched external standard method.The results showed that the limits of detection（LODs,S/N〉3）for the nine neonicotinoid insecticides were in the range of 0.3-0.8μg/kg,and the limits of quantitation（LOQs,S/N〉10）were in the range of 1.0-2.5μg/kg with good linearity（r^2〉0.9969）achieved.The average recoveries were in the range of 81.7%-106.7% for the nine residues with the relative standard deviations（RSDs）ranging from 4.2%to 9.4%at the spiked levels of 2.5,10 and 25μg/kg in multifloral,rape,cotton and sunflower honey.The method is rapid and simple with high sensitivity and good reproducibility,and suitable for the determination of the neonicotinoid insecticides in honey.