QuEChERS-高效液相色谱串联质谱法测定甜橙中哒螨灵和螺螨酯  

Simultaneous Analysis of Pyridaben and Spirodiclofen Residues in Orange Using QuEChERS-HPLC-MS/MS Technology

作　　者：滕菲菲 徐永丙 朴秀英 涂晓慧 朱献文 刘一璇 赵文婷[2] 贾明宏[2] TENG Fei-fei;XU Yong-bing;PIAO Xiu-ying;TU Xiao-hui;ZHU Xian-wen;LIU Yi-xuan;ZHAO Wen-ting;JIA Ming-hong(College of Food Science and Engineering,Beijing University of Agriculture,Beijing 102206,China;College of Biological and Resources Environment,Beijing University of Agriculture,Beijing 102206,China;Institute for the Control of Agrochemicals,Ministry of Agriculture and Rural Affairs,P.R.of China,Beijing 102206,China;HOPE Analytech Inc,Nanjing 210046,China;Jiantong Biotechnology Co.,Ltd.,Tianjin 300457,China)

机构地区：[1]北京农学院食品科学与工程学院,北京102206 [2]北京农学院生物与环境资源学院,北京102206 [3]农业农村部农药检定所,北京102206 [4]江苏衡谱分析检测技术有限公司,南京210046 [5]天津检通生物技术有限公司,天津300457

出　　处：《农药》2020年第5期367-371,共5页Agrochemicals

基　　金：国家重点研发计划资助(2017YFD0200304);北京市自然科学基金青年项目(2194072)。

摘　　要：[目的]建立了甜橙全果、果肉、果皮、果渣、橙汁和精油等6项基质中哒螨灵和螺螨酯的QuEChERS-高效液相色谱-串联质谱分析检测方法(HPLC-MS/MS)。[方法]甜橙样品经乙腈提取,PSA、GCB、MgSO4净化,高效液相色谱-串联质谱仪配备电喷雾正离子多反应监测(MRM),外标法定量。[结果]甜橙6种基质通过此分析检测方法,哒螨灵和螺螨酯在0.001~1.25 mg/L质量浓度范围线性相关系数不小于0.9965,3个加标水平(0.01、0.5、5 mg/kg)下哒螨灵回收率为81%~93%,RSD为0.5%~6.5%,螺螨酯回收率为81%~99%,RSD为0.5%~7.9%。[结论]该方法简单、方便、灵敏度、准确度高,覆盖甜橙全项样品基质,可适用于大批量样品快速分析。[Aims]This study aims to develop a QuEChERS-HPLC-MS/MS method for analysis of pyridaben and spirodiclofen in six orange by-products including whole fruit,pulp,peel,pomace,orange juice and essential oil.[Methods]The sweet orange samples was extracted with acetonitrile and purified with PSA,GCB and MgSO4,followed by electrospray positive ion multireaction monitoring(MRM)and quantitative measurement by means of external standard method.[Results]The results showed that the amount of pyridaben and spirodiclofen in the six by-products ranged from 0.001 to 1.25 mg/L with the linear coefficient higher than 0.9965 at three spiked levels(0.01,0.5,5 mg/kg).The recovery rate of pyridaben is from 81 to 93% with RSD ranging from 0.5 to 6.5%,and the recovery rate of spirodiclofen is from 81 to 99% with RSD ranging from 0.5 to 7.9%.[Conclusions]In conclusion,this method is simple,convenient,sensitive and accurate,and can be used for measurement of all by-products of sweet orange,and for rapid analysis of large samples.

关 键 词：甜橙 哒螨灵 螺螨酯 QUECHERS 高效液相色谱-串联质谱法 

分 类 号：TQ450.2[化学工程—农药化工]