氟吡菌胺及其代谢物2,6-二氯苯甲酰胺在马铃薯中残留量检测

目的]建立了以QuEChERS为样品前处理方法的超高效液相色谱串联质谱快速检测马铃薯中氟吡菌胺和2,6-二氯苯甲酰胺残留的分析方法。方法]样品经乙腈提取,PSA净化,电喷雾电离、正离子模式采集,多反应监测模式检测,基质匹配标准品外标法定量。结果]在0.01~1 mg/L范围内,氟吡菌胺和2,6-二氯苯甲酰胺在马铃薯中的质量浓度与对应的峰面积间呈良好的线性关系,其相关系数均大于0.9982。在0.01~0.5 mg/kg添加水平下,氟吡菌胺和2,6-二氯苯甲酰胺在马铃薯中的平均回收率为85.1%~97.3%,相对标准偏差(RSD)为0.8%~10.6%。氟吡菌胺和2,6-二氯苯甲酰胺在马铃薯中的定量限(LOQ)均为0.01 mg/kg。结论]该方法简便、快速、准确,可用于马铃薯中氟吡菌胺和2,6-二氯苯甲酰胺的残留检测。12地试验最终马铃薯样品中氟吡菌胺残留量均低于我国规定的最大残留限量(0.05 mg/kg)。

Residues of Fluopicolide and Its Metabolite 2,6-Dichlorobenzamide in Potato

Aims]A rapid and sensitive analytical method for the determination of fluopicolide and 2,6-dichlorobenzamide residues in potato was established based on Qu EChERS(quick,easy,cheap,effective,rugged and safe)and high performance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS).Methods]The samples were extracted with acetonitrile,and purified with primary secondary amine(PSA).The mass spectrometer was performed in multi-reaction monitoring mode,and electrospray ionization in positive mode was selected.The fluopicolide and 2,6-dichlorobenzamide residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect.Results]The results indicated that the calibration curves of fluopicolide and 2,6-dichlorobenzamide were linear in the range of 0.01-1 mg/L with correlation coefficients of more than 0.9982.When the addition level ranged from 0.01 to 0.5 mg/kg,the average recoveries of fluopicolide and 2,6-dichlorobenzamide in potato were 85.1-97.3%,and the relative standard deviation(RSD)ranged from 0.8 to 10.6%.The limit of quantitation(LOQ)of fluopicolide and 2,6-dichlorobenzamide were 0.01 mg/kg in potato.Conclusions]This method is simple,rapid and accurate,and can be adapted for the confirmation of fluopicolide and 2,6-dichlorobenzamide residues in potato samples.The results of twelve locations revealed that the fluopicolide residues in potato were less than the MRL set by China(0.05 mg/kg).