建立了液相色谱–串联质谱测定苹果、甘蓝和番茄中的溴氰虫酰胺的残留检测方法。样品经过改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)方法提取,采用乙腈提取,NaCl盐析,PSA净化,以Agilent Zarbax SB C18色谱分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子(ESI+)多反应模式监测,液相色谱–串联质谱测定。在本方法条件下,溴氰虫酰胺在0.025~5.0μg/m L浓度范围内均呈现良好的线性关系(R~2〉0.996),检测限和定量限分别为0.0015和0.005 mg/kg。在0.005、0.05和0.5 mg/kg三个添加水平下,溴氰虫酰胺在苹果、甘蓝和番茄中日内平均回收率75.44%~89.76%,日内相对标准偏差为2.32%~7.56%;日间平均回收率80.70%~93.05%,日间相对标准偏差为3.40%~11.96%,能满足苹果、甘蓝和番茄中溴氰虫酰胺检测的要求。
A novel method was developed for rapid determination of cyantraniliprole in apple, cabbage and tomato by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The sample was prepared by using a modified QuEChERS method to extract the target analyte. In this modified QuEChERS method, sample was extracted with acetonitrile, then salted out with NaC1, purified with PSA, separated on an Agilent Zarbax SB C18 column with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluant, and detected by LC-MS/MS under positive electrospray ionization (ESI+) and multiple-reaction monitoring (MRM) models. The results show that,under these conditions, cyantraniliprole has a good linearity in the concentration range of 0.025-5.0 p.g/mL with R2 〉 0.996, and the limits of detection and quantification are 0.0015 mg/kg and 0.005 mg/kg, respectively. When three spiked levels of cyantraniliprole in apple, cabbage and tomato are 0.005 mg/kg, 0.05 mg/kg and 0.5 mg/kg ,the intra-day average recoveries of cyantraniliprole are form 75.44% to 89.76% with intra-day relative standard deviations (RSDs) of 2.32%-7.56%; the inter-day average recoveries are from 80.70% to 93.05% with inter-day RSDs of 3.40%-11.96%, which can meet the requirements of cyantraniliprole determination in apple, cabbage and tomato.