QuEChERS-液相色谱-串联质谱法同时测定蔬菜中7种新烟碱类农药

Simultaneous determination of 7 neonicotinoid pesticides in vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry

[目的]建立一种同时测定蔬菜中7种新烟碱类农药残留量的分析方法。[方法]样品采用1%酸化乙腈提取,QuEChERS前处理方法,结合液相色谱-串联质谱法(LC-MS/MS)进行定性定量测定。[结果]7种新烟碱类农药在0.5~20.0μg/L质量浓度范围内呈良好的线性关系,相关系数r的范围为0.998 96~0.999 92,方法检出限(LOD)和定量限(LOQ)分别为1.0、2.0μg/kg。在韭菜、黄瓜、芹菜3种基质中,进行1、2、10μg/kg 3个水平的加标试验,平均回收率为70.6%~122.6%,相对标准偏差(RSD)为2.0%~8.8%。[结论]该方法操作简单快捷,具有较高的灵敏度、准确度和精密度,且可同时测定多种新烟碱类农药,适用于批量蔬菜样品的测定,具有较高的实际应用意义。

[Aims]Establishing an analytical method for simultaneous determination of 7 neonicotinoid pesticides residues in vegetables.[Methods]The samples were extracted by 1%acidified acetonitrile,pre-treated by QuEChERS,and qualitatively and quantitatively determined by LC-MS/MS.[Results]The seven neonicotinoid pesticides showed a good linear relationship in the concentration range from 0.5 to 20.0μg/L,the correlation coefficient r ranged from 0.99896 to 0.99992.The limit of detection(LOD)was 1.0μg/kg and the limit of quantification(LOQ)was 2.0μg/kg.The average recovery was 70.6%-122.6%and the relative standard deviation(RSD)was 2.0%-8.8%at 3 spiked levels of 1,2 and 10μg/kg in leek,cucumber and celery substrates.[Conclusions]The method is simple and fast in operation,has high sensitivity,accuracy and precision,and can simultaneously determine a variety of neonicotinoid pesticides.It is suitable for the determination of batch vegetable samples,and has high practical significance.