超高效液相色谱-串联质谱法检测番茄和甘蓝中溴虫氟苯双酰胺的残留

Simultaneous Determination of Broflanilide Residues in Tomato and Cabbage by UPLC-MS/MS

[目的]利用超高效液相色谱-串联质谱建立番茄和甘蓝中溴虫氟苯双酰胺残留量测定的方法。[方法]样品用酸化乙腈提取,N-丙基乙二胺分散吸附剂净化,超高效液相色谱分离,三重四级杆串联质谱检测,外标法定量。[结果]溴虫氟苯双酰胺在0.0002～0.2 mg/L质量浓度范围内呈现出良好的线性关系(r>0.999),当添加质量分数为0.01～0.5 mg/kg时,溴虫氟苯双酰胺在番茄中的平均回收率为71.9%～97.3%,相对标准偏差为3.2%～4.1%;在甘蓝中的平均回收率为77.5%～117.5%,相对标准偏差为6.4%～7.6%。[结论]方法的灵敏度、准确度、精密度符合农药残留分析的要求。

[Aims] A rapid and sensitive analytical method for detecting broflanilide residues in tomato and cabbage samples was established.[Methods ] The sample was extracted with acid acetonitrile, subsequently cleaned-up with primary secondary amine prior to sample analysis. UPLC-MS/MS operated on positive ionization and detected in multi-reaction monitoring model, quantitative by external standard method.[Results] The method showed excellent linearity (r>0.999) for broflanilide in the range of 0.0002-0.02 mg/L. Recovery studies were performed at spiked levels of 0.01-0.5 mg/kg. Recoveries of the method ranged from 71.9 to 97.3% with relative standard deviation (RSD) ranged from 3.2 to 4.1% for tomato at different levels. Recoveries for cabbage at different levels ranged from 77.5 to 117.5% with RSD ranged from 6.4 to 7.6%.[Conclusions ] The method was simple and reliable, meet with the requirement of pesticide residues analysis, and could be applied for determining broflanilide in tomato and cabbage.