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Simultaneous determination of pyflubumide and its metabolite in vegetables and fruits by ultrahigh performance liquid chromatography-tandem mass spectrometry
Authors:Wei Zuo  Chao Dong  Bining Jiao  Chengqiu Wang  Jing Li
Institution:1. Citrus Research Institute, Southwest University, Chongqing, P. R. China;2. Citrus Research Institute, Southwest University, Chongqing, P. R. China

Laboratory of Citrus Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture and Rural Affairs, Chongqing, P. R. China

Quality Supervision and Testing Center for Citrus and Seedling, Ministry of Agriculture and Rural Affairs, Chongqing, P. R. China

Abstract:A rapid and cost-effective analytical method based on ultrahigh-performance liquid chromatography-tandem mass spectrometry was designed and verified for simultaneously monitoring the novel acaricide pyflubumide and its metabolite (pyflubumide-des(2-methyl-1oxopropyl)) in vegetables and fruits. After the extraction with acetonitrile, the samples were purified by dispersive solid-phase extraction with multi-walled carbon nanotubes. Detection of the two target analytes was achieved within 3.0 min using a positive electrospray ionization mode. The average recovery, intra-day precision, and inter-day precision of the two analytes at three spiked levels (2, 20, and 100 μg/kg) were 75.0–101.0, 0.4–4.4, and 0.6–5.3%, respectively. The limit of quantification of two compounds was 2 μg/kg, which was far below the maximum residue limits of pyflubumide in foods established by Japan and South Korea. Finally, the concentrations of pyflubumide and its metabolite in the samples were 16.6 and 7.8 μg/kg respectively, which verified the practicability and reliability of the method. The method was used to efficiently detect pyflubumide and its metabolite in real samples and was confirmed to be robust and effective for routinely analyzing both pyflubumide and its metabolite in vegetable and fruit samples.
Keywords:acaricides  metabolites  multiwalled carbon nanotubes  pesticides
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