建立一种QuEChERS前处理方法结合高效液相色谱-串联质谱（high performance liquid chromatography-tandem mass spectrometry，HPLC-MS/MS）技术同时检测荔枝龙眼基质中苯醚甲环唑、氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38残留量的分析方法。荔枝龙眼基质样品采用乙腈作为提取溶剂，利用50 mg十八烷基键合硅胶（C18）、50 mg N-丙基乙二胺（PSA）和10 mg纳米氧化锆（Nano-ZrO2）3种吸附剂联合净化，用75 mm InfinityLab Poroshell 120 SB-C18色谱柱进行分离，并以0.1%（体积分数）甲酸水溶液-乙腈为流动相进行梯度洗脱，多反应离子监测模式（MRM）扫描，以基质匹配标准溶液进行定量分析。结果显示：4种目标化合物在1~100 μg/kg质量浓度范围内线性相关系数为0.9896~0.9999，定量限（LOQ）为0.10~10 μg/kg。荔枝龙眼中4种目标分析物的加标回收率为82.48%~99.17%，日内和日间相对标准偏差分别为4.11%~7.77%、6.10%~13.27%。本方法具有易于操作、简便快速和灵敏度高等优势，可应用于荔枝龙眼实际样品中苯醚甲环唑、氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38残留的同时检测分析。

An analytical method was established for the determination of difenoconazole, chlorantraniliprole, cyantraniliprole and their metabolite J9Z38 residues in litchi and longan by QuEChERS pretreatment method with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) technique. Residues in litchi and longan samples were extracted with acetonitrile, purified with 50 mg C18, 50 mg PSA, and 10 mg Nano-ZrO2, and then detected by HPLC-MS/MS with separation column of 75 mm InfinityLab Poroshell 120 SB-C18, and 0.1% formic acid-acetonitrile as mobile phase with gradient elution under multi-reactive ion monitoring (MRM) and quantified by external matrix-matched standard. Good linearities for the four analytes in the range of 1~100 μg/kg were obtained and the correlation coefficients (r2) were from 0.9896 to 0.9999. The limits of quantitation (LOQs) were among 0.10 to 10 μg/kg. The recoveries in the litchi and longan were ranged from 82.48% to 99.17%, the intra-day precisions and inter-day precisions were 4.11%~7.77% and 6.10%~13.27%, respectively. The developed method have several advantages: easy to operate, simple and rapid, and high sensitivity. The method can be used for monitoring of difenoconazole, chlorantraniliprole, cyantraniliprole and their metabolite J9Z38 in real litchi and longan samples.

广东省乡村振兴战略专项项目（403-2018-XMZC-0002-90）；广州市科技计划项目（202102080338）；国家荔枝龙眼产业技术体系项目（CARS-32-15）；广东省农业科学院院长基金项目（201929；202026）