滤过型净化柱结合HPLC-MS/MS测定蜂花粉中9种农药

Simultaneous Determination of Nine Pesticide Residues in Bee Pollen Using Multiplug Filtration Cleanup Coupled HPLC-MS/MS

[目的]建立一种同时测定蜂花粉中9种农药残留的高效、快速分析方法。[方法]蜂花粉样品经乙腈/水提取,-80℃冷冻4 min,上清液经多壁碳纳米管滤过型净化柱进行2次反复抽提净化,采用正离子多反应监测MRM模式进行分析,外标法定量。[结果]该方法线性良好,R2均大于0.99,9种农药的加标回收率在80.5%~106.2%之间,相对标准偏差(RSD)小于11.1%,定量限(LOQ)均为0.01 mg/kg,蝇毒磷和毒死蜱除外,为0.1 mg/kg。[结论]该方法操作简单,准确度、精密度、灵敏度均能满足方法要求,适用于蜂花粉中9种农药残留同时快速检测。

[Aims]This study aims to establish an analytical method for simultaneous residue determination of nine pesticides in bee pollen.[Methods]Samples were extracted with acetonitrile/water,freezed at-80℃for 4 min,cleaned up by 2 times multiplug filters containing carbon manotubes(m-PFC),and then determined by HPLC-MS/MS operated in positive multiple reaction monitoring(MRM).[Results]The results showed a good linear relationship was achieved with linear correlation coefficients(R2)higher than 0.99.The mean recoveries of the 9 pesticides were 80.5-106.2%,with relative standard deviations(RSD)of less than 11.1%.The limits of quantitation(LOQ)were 0.01 mg/kg,except for coumaphos and chlorpyrifos(0.1 mg/kg)in bee pollen.[Conclusions]The results indicated this method is reliable for monitoring the nine pesticide residues in bee pollen.