QuEChERS-高效液相色谱-串联质谱法测定毛豆中常用21种农药残留

目的建立液相色谱-串联质谱法同时检测毛豆中21种常用农药残留的分析方法。方法样品以乙腈-甲酸(99:1,V:V)作为提取剂,经Qu ECh ERS方法前处理,采用Phenomenex的Kinetex C_(18)色谱柱(50 mm×2.1mm,2.6μm,100?)分离,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,以电喷雾电离(ESI)、正离子模式和负离子模式2种多反应监测(MRM)模式检测,外标法定量。结果 21种农药在5~200 ng/m L范围内,线性相关系数均大于0.99,线性良好。分析目标物添加水平为0.01~0.10 mg/kg时,回收率范围为73%~113%,RSD范围为1.3%~10.9%,符合残留分析的要求。21种农药的定量下限为0.01 mg/kg。结论该方法的提取简便,基质分散效果好,灵敏度满足国内外限量标准的要求,适合毛豆中常用农药残留的同时测定。

Determination of 21 kinds of pesticide residues in soybean by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

This paper established a simultaneous detection of liquid chromatography - tandem mass spectrometry of 21 kinds of pesticide residues in soybean (HPLC-MS/MS) testing method. Samples with acetonitrile / formic acid (99/1, V/V) as extraction agent, were performed by QuEchERS method, using Kinetex C18 Phenomenex chromatographic column (50mm * 2.1mm, 2.6um, 100A) to separate. Gradient elution with acetonitrile and 0.1% formic acid was the mobile phase gradient. The resulting samples were detected under positive and negative multiple reactions monitoring (MRM) mode,and quantified by external standard method. With the 21 kinds of pesticides in the range of 5~200ng/mL, the linear correlation coefficient was greater than 0.99, with good linearity. Analysis of the target addition level was 0.01~0.10mg/kg, the recovery rate was in the range of 88%~113%, the RSD range of 4.3%~10.8%, in accordance with the requirements of residue analysis. The limits of determination and the limits of quantification of the 21 pesticides was 0.01-0.005mg/kg. The method is quick, easy, effective, sensitive and accurate, and can meet the requirements for the determination of for the simultaneous determination of pesticide residues in Vegetable Soybean Used.