UPLC-MS/MS测定棉铃虫体内丁布的残留量

【目的】对比2种前处理方法对丁布含量的影响,建立UPLC-MS/MS测定棉铃虫体内丁布含量的分析方法。【方法】棉铃虫样品经甲醇涡旋振荡、超声波提取,用Waters UPLC-MS/MS (Xevo TQS质谱)检测丁布的含量,BEH C₁₈色谱柱,流动相为甲醇-水(含0.5%的冰乙酸)梯度洗脱,流速0.3 mL/min。【结果】棉铃虫样品在低浓度5 μg/L、高浓度50 μg/L 2个添加水平下,甲醇超声提取法的添加回收率最佳,平均添加回收率分别为84.26%、96.78%,最低检测质量浓度为5 μg/L。【结论】该方法的准确度和精密度、添加回收率均符合化合物残留分析的要求。

Determination of DIMBOA Residues in Helicoverpa armigera by UPLC-MS/MS

【Objective】 To compared the effects of two pretreatment methods on the determination of DIMBOA in Helicoverpa armigera, and establish an UPLC-MS/MS method for the determination of DIMBOA in H. armigera. 【Methods】 The samples of H. armigera were extracted by methanol vortex oscillation and ultrasonic wave and the content of DIMBOA was determined by Waters UPLC-MS/MS (Xevo TQS mass spectrometry). The chromatographic column was BEH C18, the mobile phase was methanol- pure water (containing 0.5% glacial acetic acid) gradient elution, and the flow rate was 0.3 mL/min. 【Results】 At concentrations of 5 and 50 μg/L, the addition recovery rate of methanol ultrasonic extraction method was the best, the average addition recovery rates were 84.26% and 96.78%, respectively, and the limit of quantity was 5 μg/L. 【Conclusion】 The accuracy, precision and addition recovery of methanol ultrasonic extraction method meet the requirements of compound residue analysis.