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Solid‐phase extraction combined with dispersive liquid–liquid microextraction for the determination of pyrethroid pesticides in wheat and maize samples
Authors:Xiaodan Zhu  Chunhong Jia  Zuntao Zheng  Xiaoyuan Feng  Yue He  Ercheng Zhao
Affiliation:1. Institute of Plant and Environment Protection, Beijing Academy of Agriculture and Forestry Science, Beijing, China;2. Beijing Research Center for Agricultural Standards and Testing, Beijing, China;3. Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing, China
Abstract:A rapid, selective and sensitive sample preparation method based on solid‐phase extraction combined with the dispersive liquid–liquid microextration was developed for the determination of pyrethroid pesticides in wheat and maize samples. Initially, the samples were extracted with acetonitrile and water solution followed phase separation with the salt addition. The following sample preparation involves a solid‐phase extraction and dispersive liquid–liquid microextraction step, which effectively provide cleanup and enrichment effects. The main experimental factors affecting the performance both of solid‐phase extraction and dispersive liquid–liquid microextration were investigated. The validation results indicated the suitability of the proposed method for routine analyze of pyrethroid pesticides in wheat and maize samples. The fortified recoveries at three levels ranged between 76.4 and 109.8% with relative standard deviations of less than 10.7%. The limit of quantification of the proposed method was below 0.0125 mg/kg for the pyrethoroid pesticides. The proposed method was successfully used for the rapid determination of pyrethroid residues in real wheat and maize samples from crop field in Beijing, China.
Keywords:Dispersive liquid–  liquid microextraction  Insecticides  Sample preparation  Solid‐phase extraction
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