QuEChERS-超高效液相色谱-串联质谱法同时测定芒果中氟吡菌酰胺、肟菌酯及其代谢物残留量  

Determination of Fluopyram,Trifloxystrobin and Its Metabolite in Mango by QuEChERS-UHPLC-MS/MS

作　　者：范金平 张盈[2] 魏进[2] 罗世霞[1] 段婷婷[2] FAN Jin-ping;ZHANG Ying;WEI Jin;LUO Shi-xia;DUAN Ting-ting(College of Chemistry and Materials Science,Guizhou Normal University,Guiyang 550025,China;State Key Laboratory for Biology of Plant Diseases and Insect Pests,Institute of Plant Protection,Guizhou Academy of Agricultural Sciences,Guiyang 550009,China)

机构地区：[1]贵州师范大学化学与材料科学学院,贵阳550025 [2]贵州省农业科学院植物保护研究所,贵阳550009

出　　处：《农药》2020年第7期516-522,共7页Agrochemicals

摘　　要：[目的]建立超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时检测氟吡菌酰胺及其代谢物2-(三氟甲基)苯甲酰胺、肟菌酯及其代谢物肟菌酸在芒果皮、芒果肉中残留分析检测方法。[方法]芒果样品经1%乙酸乙腈提取,50.00 mg C18+10.00 mg GCB净化,乙腈和0.1%甲酸水作为流动相梯度洗脱,C18色谱柱分离,氟吡菌酰胺及其代谢物2-(三氟甲基)苯甲酰胺、肟菌酯及其代谢物肟菌酸采用电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,基质标准溶液外标法定量。[结果]氟吡菌酰胺、肟菌酯及其代谢物肟菌酸溶剂标准曲线和基质标准曲线在0.25~250μg/L范围内线性良好,氟吡菌酰胺代谢物2-(三氟甲基)苯甲酰胺溶剂标准曲线和基质标准曲线在2.50~250.00μg/L范围内线性关系良好。在0.0005、0.005、0.05 mg/kg 3个添加质量分数下,方法的回收率为88.7%~105.2%,相对标准偏差为2.5%~7.0%。氟吡菌酰胺、肟菌酯、肟菌酸的方法定量限为0.0005 mg/kg,2-(三氟甲基)苯甲酰胺定量限为0.005 mg/kg。[结论]该方法操作简单、灵敏度高、准确可靠,适用于芒果皮、芒果肉中2种杀菌剂及其代谢物残留量的同时检测,为解决氟吡菌酰胺及其代谢物、肟菌酯及其代谢物在食品中残留的安全问题提供技术支撑。[Aims]This study aims to establish a method for simultaneous determination of fluopyram and its metabolite 2-(trifluoromethyl)benzamid,trifloxystrobin and its metabolite trifloxystrobin acid in mango skin and flesh samples by ultra performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).[Methods]The experimental samples were extracted with acetonitrile containing 1%acetic acid and purified with 50.00 mg C18 and 10.00 mg GCB.The mobile phase was eluted with acetonitrile and 0.1%formic acid aqueous solution.The analyte was separated on an ACQUITY UPLC HSS C18 column and quantitatively analyzed by the external standard method using matrix-matched calibration curves.[Results]There were good linearity in the range of 0.25-250.00μg/L under the optimal conditions.The spiked recoveries of 2 fungicides and their metabolites in mango skin and flesh at three spiked levels of 0.0005,0.005,0.05 mg/kg ranged from 88.7 to 105.2%,with relative standard deviations RSDs of 2.5-7.0%.The limits of quantitation of LOQ were 0.0005-0.005 mg/kg.[Conclusions]The established method was simple,sensitive,accurate and reliable and could meet the requirement of multi pesticide residues analysis in mango skin and flesh.It was of great significance to solve the safety problems for the residue of fluopyram and its metabolite,trifloxystrobin and its metabolite in foods.

关 键 词：氟吡菌酰胺 肟菌酯 代谢物 芒果 QUECHERS 超高效液相色谱-串联质谱 

分 类 号：TQ450.2[化学工程—农药化工]