QuEChERS结合超高效液相色谱-串联质谱法同时测定果蔬中12种新烟碱类农药残留

Simultaneous determination of 12 kinds of neonicotinoid pesticides in fruits and vegetables by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  新烟碱类农药  果蔬  QuEChERS法  超高效液相色谱-串联质谱法  基质效应

英文关键词:neonicotinoid pesticides  fruit and vegetable  QuEChERS method  ultra performance liquid chromatography-tandem mass spectrometry  matrix effect

中文摘要:

      目的 建立基于QuEChERS前处理技术结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测水果和蔬菜中12种新烟碱类农药残留的分析方法。方法 样品采用乙腈提取, 上清液采用N-丙基乙二胺、无水硫酸镁(MgSO4)和石墨化炭黑的QuEChERS基质分散萃取法净化, 经InfinityLab Poroshell 120 EC-C18 (100 mm×2.1 mm, 2.7 μm)色谱柱分离, 以0.1%甲酸水溶液(含5 mmoL/L乙酸铵)-乙腈为流动相, 基质匹配曲线外标法定量。结果 12种新烟碱类农药在0.05~200.00 ng/mL范围内具有良好的线性关系(r2>0.99), 方法检出限(S/N=3)为0.02~0.26 μg/kg。在2.0、20.0、50.0 μg/kg加标水平下的平均回收率为88.90%~118.00%, 相对标准偏差(relative standard deviations, RSDs, n=6)为1.55%~6.12%。在6种果蔬基质中, 12种目标物存在不同的基质效应。与国家标准方法比较发现, 在3种色素含量较高的果蔬基质中, 本方法的回收率高于标准方法回收率, 且其RSD小于标准方法的RSD。结论 该方法提取效果好、灵敏度高、专属性强, 适用于果蔬中12种新烟碱类农药残留快速检测及确证分析。

英文摘要:

      Objective To establish a method for the simultaneous determination of 12 kinds of neonicotinoid pesticides residues in fruits and vegetables by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on QuEChERS pretreatment technique. Methods The sample was extracted with acetonitrile. The supernatant was purified using a QuEChERS matrix dispersion extraction method of N-propylethylenediamine, anhydrous magnesium sulfate (MgSO4), and graphitized carbon black, and then subjected to InfinityLab Poroshell 120 EC-C18 (100 mm×2.1 mm, 2.7 μm) chromatographic column for separation, using 0.1% formic acid aqueous solution (containing 5 mmoL/L ammonium acetate) -acetonitrile as mobile phase, and matrix matching curve external standard method was used for quantitative analysis. Results The 12 kinds of neonicotinoid pesticides had good linear relationship in the range of 0.05?200.00 ng/mL (r2>0.99), and the limit of detection (S/N=3) was 0.02?0.26 μg/kg. The average recoveries at levels of 2.0, 20.0, 50.0 μg/kg were 88.90% to 118.00%, and the relative standard deviations (RSDs, n=6) was 1.55%?6.12%. Among the 6 kinds of fruit and vegetable substrates, 12 kinds of target substances had different matrix effects. Compared with the national standard method, among the 3 fruit and vegetable substrates with high pigment content, the recoveries of this method was higher than that of the standard method, and the RSD was smaller than that of the standard method. Conclusion This method has good extraction effect, high sensitivity and strong specificity, and is suitable for rapid detection and confirmatory analysis of 12 kinds of neonicotinoid pesticide residues in fruits and vegetables.