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A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues
Authors:Qiuhong Yang  Xiaohui Ai  Jing Dong  Yongtao Liu  Shun Zhou  Yibin Yang  Ning Xu
Institution:1.Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan 430223, China; (J.D.); (Y.L.); (S.Z.); (Y.Y.); (N.X.);2.Chinese Academy of Fishery Sciences, Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing 100141, China
Abstract:We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.
Keywords:QuEChERS  HPLC-MS/MS  Imidacloprid  metabolites  5-hydroxy imidacloprid  olefin imidacloprid  Imidacloprid urea  6-chloronicotinic acid  Procambarus clarkii
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