QuEChERS结合高效液相色谱-串联质谱同时测定荔枝龙眼中3种农药及代谢物残留

Simultaneous Determination of Three Pesticides and Their Metabolite Residues in Litchi and Longan by High Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS

摘要:

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。

Abstract:

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.