超高效液相色谱-三重四极杆串联质谱法测定柑橘中4种苯甲酰脲类农药残留

建立了柑橘中虱螨脲、灭幼脲、氟啶脲和除虫脲4种苯甲酰脲类农药同时检测的超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)分析方法。样品采用QuEChERS前处理技术,超高效液相色谱-串联质谱电喷雾负离子模式检测测定。结果表明:在0.01~0.2μg/mL范围内,4种供试农药的质量浓度与其相应的峰面积间呈良好的线性关系,相关系数(r)均大于0.994。在0.01、0.05和0.1 mg/kg 3个添加水平下,4种农药的平均回收率为92%~105%,相对标准偏差(RSD)为0.4%~3.3%(n=5)。4种农药在柑橘中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、简单,适用于同时测定柑橘中4种苯甲酰脲类农药的残留量。

Determining residues of 4 benzoylurea pesticides in citrus fruits by ultra performance liquid chromatography-tandem mass spectrometry

A ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method for the simultaneous determination of 4 benzoylurea pesticides (lufenuron, chlorbenzuron, chlorfluazuron and diflubenzuron) in citrus fruits was established. The procedure was based on QuEChERS cleanup and determination with UPLC-MS/MS. The results showed that the calibration curve was linear in the range of 0.01-0.2 mg/mL and correlation coefficient(r) higher than 0.994. The average recoveries of 4 pesticides were 92%-105% when the spiked levels were 0.01, 0.05 and 0.1 mg/kg, with relative standard deviations (RSD) between 0.4% and 3.3% (n=5). The limits of quantitation (LOQ) for 4 pesticides were 0.01 mg/kg. The method is accurate, sensitive, simple, suitable for the simultaneous determination of 4 pesticide residues in citrus fruits.