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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 liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of residues of bromothiramide in apple, cabbage and tomato. Samples were extracted using a modified QuEChERS method (Fast, Simple, Cheap, Efficient, Flexible and Safe) using acetonitrile extraction, NaCl salting-out and PSA purification on an Agilent Zarbax SB C18 column with a gradient of acetonitrile and 0.1% formic acid Elution, electrospray positive ion (ESI +) multi-reaction mode monitoring, liquid chromatography-tandem mass spectrometry. Under the conditions of this method, a good linear relationship (R ~ 2> 0.996) was obtained for the concentration of bromothiramide in the range of 0.025-5.0μg / mL with the limits of detection and limit of quantification of 0.0015 and 0.005 mg / kg, respectively. The average recoveries of bromoxetane in apple, cabbage and tomato were 75.44% ~ 89.76% at three levels of 0.005, 0.05 and 0.5 mg / kg, respectively. The relative standard deviations were 2.32% ~ 7.56% The recoveries ranged from 80.70% to 93.05%, and the relative standard deviations (RSDs) ranged from 3.40% to 11.96% during the day, which could meet the requirements of bromoxetane detection in apple, cabbage and tomato.