QuEChERS净化结合超高效液相色谱串联质谱法快速测定动物源性食品中溴虫氟苯双酰胺残留

Rapid determination of broflanilide residues in animal-derived foods by QuEChERS purification combined with UPLC-MS/MS

该研究建立了一种QuEChERS净化结合超高效液相色谱串联质谱法(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)快速测定动物源性食品中溴虫氟苯双酰胺残留量的分析方法。样品使用QuEChERS吸附净化,经含0.1%(体积分数)甲酸的乙腈提取,MgSO_(4)、C18及N-丙基乙二胺净化,净化液离心后过膜上机测定。UPLC-MS/MS法以乙腈和5 mmol/L乙酸铵(含体积分数0.1%甲酸)水溶液为流动相,以0.300 mL/min的流速进行梯度洗脱,使用ACQUITY UPLC BEH C18色谱柱进行分离,电喷雾离子源正离子模式电离,多反应监测模式检测,基质匹配标准曲线外标法定量。结果表明:溴虫氟苯双酰胺在0.200~100μg/L范围内呈良好线性,相关系数(R^(2))均大于0.999,方法的定量限为0.5~1.0μg/kg;以动物源性食品为基质,在低中高(2.0、10.0和50.0μg/kg)添加水平下,溴虫氟苯双酰胺的平均加标回收率为93.9%~102%,相对标准偏差为2.25%~5.86%。该方法便于操作,实验过程短,检测准确性高,可以填补动物源性食品中溴虫氟苯双酰胺的检测方法的空白,并可为动物源性食品中溴虫氟苯双酰胺农药残留限量值的制定提供技术支撑。

In this study,a QuEChERS purification combined with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for the rapid quantification of broflanilide residues in animal-derived food.The samples were extracted and purified using the QuEChERS method,followed by extraction with acetonitrile containing 0.1%formic acid.The extract was subsequently purified using anhydrous magnesium sulfate,C18,and primary secondary amine,followed by centrifugation and membrane filtration prior to analysis.The UPLC-MS/MS method utilized acetonitrile and a 5 mmol/L ammonium acetate solution with 0.1%formic acid as the mobile phase,with a flow rate of 0.300 mL/min for gradient elution.Separation was achieved using an ACQUITY UPLC BEH C18 column,and electrospray ionization in positive ion mode was employed for ionization.The detection was performed in multiple reaction monitoring mode,and quantification was performed using the external standard method with matrix-matched standard curves.The results demonstrated that broflanilide residues displayed excellent linearity within the range of 0.200 to 100μg/L,with correlation coefficients(R^(2))all exceeding 0.999.The method’s limits of quantification were 0.5-1.0μg/kg.When animal-derived food was used as the matrix,at low,medium,and high spiked levels(2.0,10.0,and 50.0μg/kg),the average recovery rates for broflanilide residues ranged from 93.9%to 102%,with relative standard deviations ranging from 2.25%to 5.86%.The method is user-friendly,the experimental process is concise,and the detection accuracy is exceptional.It addresses the current gap in detecting broflanilide in animal-derived food,and offers technical support for establishing pesticide residue limits for broflanilide in animal-derived food.