超高效液相色谱串联质谱法测定豇豆中新烟碱类农药残留

Determination of residues of neonicotinoid insecticides in cowpeas by UPLC-MS/MS

本研究建立了超高效液相色谱串联质谱法(UPLC-MS/MS)同时检测豇豆中9种新烟碱类杀虫剂的多残留分析方法。豇豆样品用QuEChERS方法前处理,用Kinetex Biphenyl色谱柱分离,以甲醇和含0.1 mmol/L甲酸铵、0.001%甲酸的水作为流动相进行梯度洗脱,使用超高效液相色谱串联质谱检测分析。定量限为0.01 mg/kg,标准工作曲线在0.001~1 mg/kg范围内表现出良好的线性关系,决定系数(R^( 2))均大于0.99。目标杀虫剂在豇豆中的平均回收率为66.9%~109.8%,相对标准偏差为1.2%~10.0%。应用该方法对某地16个农贸市场中采集的71份豇豆样本进行检测,所有样品均符合我国所规定的豇豆(或豆类)中的最大残留限量标准要求。该方法简便、准确、灵敏度高,适用于新烟碱类杀虫剂在豇豆中的残留监测。

A method was developed for the simultaneous determination of nine neonicotinoid insecticides in cowpea by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The cowpea samples were pretreated with QuEChERS,and separation was performed by Kinetex Biphenyl column using a gradient elution of methanol and water(0.1 mmol/L ammonium formate+0.001%formic acid)as mobile phases,and then detected by UPLC-MS/MS.The limit of quantification(LOQ)for neonicotinoid insecticides was 0.01 mg/kg.The method showed excellent linearity(R^( 2)>0.99)in the range of 0.001-1 mg/kg.The average recoveries of the target compounds in cowpea ranged from 66.9%to 109.8%,and the relative standard deviation(RSDs)was from 1.2%to 10.0%.This method was used for determination of 71 cowpea samples collected in 16 markets and all pesticides met the requirements of the maximum residue limit standard in cowpeas(or beans)stipulated in the National Food Safety Standard Maximum Residue Limits of Pesticides in Food(GB 2763-2021).This method is simple,accurate and sensitive,and suitable for the residue analysis of neonicotinoid insecticides in cowpeas.