摘要
本研究建立了一种经过衍生化处理,测定平菇中吡虫啉及其含6-氯-吡啶基代谢物残留总量的气相色谱-串联质谱(GC-MS/MS)检测方法。样品中吡虫啉及其代谢物在碱性KMnO_(4)溶液和70℃水浴条件下氧化反应为6-氯-吡啶基的代谢物,再加入强氧化剂进一步转化为6-氯烟酸三甲基硅酯,采用多反应监测模式分析,外标法定量测定衍生物。结果表明,在0.002~0.2 mg/L范围内,吡虫啉的衍生物6-氯烟酸三甲基硅酯的质量浓度与其峰面积呈良好的线性关系(R^(2)≥0.999);在0.02~0.5 mg/kg添加浓度范围内,吡虫啉平均回收率为86%~95%,相对标准偏差为1.7%~4.8%。该方法操作简单,可满足同时测定吡虫啉及其含6-氯-吡啶基代谢物的检测需要,为分析食品中吡虫啉残留量提供新的思路。
A gas chromatography tandem mass spectrometry(GC-MS/MS)method with precolumn derivatization was established for the determination of imidacloprid and its metabolites containing the 6-chloropyridinyl moiety residues in Pleurotus ostreatus.Imidacloprid and its metabolite in the sample were oxidized to 6-chloropyridinyl metabolite with alkaline KMnO_(4) solution and 70℃water bath,and converted to 6-chloronicotinic acid trimethylsilyl ester with strong oxidant.The derivative procuded was quantified by external standard method with mass detector under multireaction monitoring mode.The results showed the standard curve was well linear by the correlation coefficient in the range of 0.02-0.2 mg/L(R^(2)≥0.999).Their average deviation at spiked levels of 0.02-0.5 mg/kg were 86%-95%,and the relative standard deviation of 1.7%-4.8%.The method was simple and suitable for detected imidacloprid and its 6-chloro-pyridyl metabolites,and provided a novel idea for analysing the safety problem of imidacloprid residues in food.
作者
曲滢
查欣欣
沈鹏
叶剑
王洪雷
QU Ying;ZHA Xinxin;SHEN Peng;YE Jian;WANG Honglei(Jianshu Evertest Limited Company,Nanjing210046,China;Jiangsu Pesticide Research Institute Co.,Ltd.,Nanjing210046,China)
出处
《现代农药》
CAS
2022年第6期47-50,共4页
MODERN AGROCHEMICALS
