超高效液相色谱-串联质谱法测定动物源食品中敌草腈及其代谢物残留

Determination of Dichlobenil and Its Metabolite Residues in Food Products of Animal Origin Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

[目的]建立一种超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定动物源食品中的敌草腈及代谢物2,6-二氯苯甲酰胺残留的方法。[方法]采用改进的QuEChERS方法进行前处理,乙腈提取,PSA净化剂与C18粉末协助净化。采用C18超高效液相色谱柱分离,流动相为乙腈和2 mmol/L乙酸铵,流速为0.25 mL/min。电喷雾正离子(ESI+)模式电离,多反应离子监测模式定性分析,外标法定量。[结果]在0.005~0.500 mg/L质量浓度范围内,线性相关系数均大于0.999,动物源样品的平均加标回收率在75%~108%,相对标准偏差(RSD)为3.7%~8.8%。敌草腈与代谢物2,6-二氯苯甲酰胺的检出限(S/N=3)分别为0.70、0.40μg/kg;定量限(S/N=10)分别为2.33、1.33μg/kg。[结论]该方法操作简便快速、灵敏、准确性高,适用于动物源食品中敌草腈与代谢物2,6-二氯苯甲酰胺的残留量检测。

[Aims]To determine the residues of dichlobenil and its metabolite residues in food products of animal origin,a method was established by using ultra-high performance liquid chromatography-tandem mass spectrometry.[Methods]The improved QuEChERS method was used for preprocessing.Acetonitrile solution extraction,PSA agent and C18 powder are used for purification.Themobile phase was acetonitrile and 2 mmol/L ammonium acetate,and the flow rate was 0.25 mL/min.Then detected by electro-spray ionization(ESI+)and multiple reaction monitoring(MRM)mode.External standard method was used for quantification.[Results]The linear correlation coefficients were all greater than 0.999 in the range of 0.005-0.500 mg/L.The mean standard recovery of samples was 75-108%,and the relative standard deviation(RSD)was 3.7-8.8%.The limit of detection(S/N=3)of dioxonitrile and 2,6-dichlorobenzamide was 0.70 and 0.40μg/kg,the limit of quantification(S/N=10)was 2.33 and 1.33μg/kg,respectively.[Conclusions]This method was quick,simple,accurate,and it was suitable for the determination of the residue of dichlobenil and 2,6-dichlorobenzamide in food products of animal origin.