QuEChERS-液相色谱-串联质谱法同时测定枸杞干果中新烟碱类农药残留

Simultaneous Determination of Neonicotinoid Pesticide Residues in Dried Lycium by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry

目的:研究同时测定枸杞中8种新烟碱类杀虫剂残留的QuEChERS-液相色谱-串联质谱-多反应监测的测试方法。方法:试样经酸化的乙腈液萃取后加盐析剂分层,提取液净化后,通过液相色谱-串联质谱正离子模式下采用多反应监测进行测定。结果:8种新烟碱类农药在2-50 ng·mL^(-1)线性关系一致,相关系数均大于0.995,方法检出限在0.01-0.09 μg·kg^(-1),本方法选择3个浓度水平进行添加回收实验,回收率分别控制在72.1%-106.8%,相对标准偏差处于0.31%-3.97%。结论:该方法快速、准确、灵敏度较高,能较好地运用于枸杞干果中新烟碱类农药残留的定性和定量检测。

Objective:To establish a method for simultaneous determination of 8 neonicotinoid pesticide residues in dried lycium by QuEChERS-liquid chromatography-tandem mass spectrometry-multi response monitoring (LC-MS/MS-MRM).Method:The samples were extracted with acidified acetonitrile solution and layered with salting-out agent.And then were purified to be detected.The diluted supernatant was passed through the membrane and determined by LC-MS/MS,using positive electrospray ionization (ESI^(+)) mode and multi MRM.Result:The linear relationship among 8 neonicotinoid pesticides were good in the concentration range of 2-50 ng·mL^(-1),with correlation coefficient over 0.995.The detection limit for all the pesticides were in the range of 0.01-0.09 μg·kg^(-1).The recoveries at three spiked levels range from 72.1% to 106.8% with relative standard devitations (RSDs) of 0.31%-3.97%.Conclusion:The method is rapid,precise and sensitive,and can be applied for the qualitative and quantitative analysis of neonicotinoid pesticide residues in dried lycium.