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

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(C_(18))、50 mg N-丙基乙二胺(PSA)和10 mg纳米氧化锆(Nano-ZrO_(2))3种吸附剂联合净化,用75 mm InfinityLab Poroshell 120 SB-C_(18)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1~100μg/kg质量浓度范围内线性相关系数为0.9896~0.9999,定量限(LOQ)为0.10~10μg/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 C_(18),50 mg PSA,and 10 mg Nano-ZrO_(2),and then detected by HPLC-MS/MS with separation column of 75 mm InfinityLab Poroshell 120 SB-C_(18),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 1~100μg/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 10μg/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.