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Hyperspeed method for analyzing organochloride pesticides in sediments using two-dimensional gas chromatography–time-of-flight mass spectrometry

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Abstract

Pesticides are traditionally analyzed using conventional gas chromatography. When fast chromatography is associated with comprehensive two-dimensional gas chromatography (GC × GC), the resulting method presents high-resolution separation associated with a higher chromatographic speed. In the present work, a method for pesticide analysis in sediment samples was developed using quick, easy, cheap, effective, rugged, and safe extraction (QuEChERS) and a hyperspeed GC × GC separation. The QuEChERS procedure reported in the literature was extended to incorporate the analytes tetrachloro-m-xylene, decachlorobiphenyl, trans-chlordane, chlordane, endosulfan lactone, and endosulfan ether. To understand the chromatographic method improvement achieved, the recent concept of average theoretical peak time (ATPT) was used. The ATPT improved from that of the traditional GC × GC separation to the proposed method, and the separation speed can be classified as a hyperspeed separation. The limit of detection and quantitation of the compounds in the standard mix ranged from 0.39 to 17.96 µg L−1 and 1.18 to 54.43 µg L−1, respectively. The method showed acceptable RSD% (relative standard deviation) values and little interference of the sediment matrix in the extraction procedure. The developed method was applied to the determination of a mixture of 19 compounds in 16 sediment samples from the Pirapetinga River and Paraíba do Sul River in Brazil.

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Funding

The authors acknowledge CAPES-Coordenação de Aperfeiçoamento de Pessoal de Nível Superior and the financial support of the Middle Paraíba do Sul Basin Committee through AGEVAP–Associação Pró-Gestão das Águas da Bacia Hidrográfica do Rio Paraíba do Sul.

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  1. Faculty of Technology, State University of Rio de Janeiro–UERJ, Polo Industrial, Rodovia Presidente Dutra, Km 298, Resende, 27537-000, Brazil

    Felipe Cury Mazza, Nilo Antônio de Souza Sampaio & Carin von Mühlen

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Published in the topical collection Comprehensive 2D Chromatography with guest editors Peter Q. Tranchida and Luigi Mondello.

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Mazza, F.C., de Souza Sampaio, N.A. & von Mühlen, C. Hyperspeed method for analyzing organochloride pesticides in sediments using two-dimensional gas chromatography–time-of-flight mass spectrometry. Anal Bioanal Chem 415, 2629–2640 (2023). https://doi.org/10.1007/s00216-022-04464-y

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