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<p>Disposable pipette extraction (DPX) is a modern miniaturized solid phase extraction technique that can be applied for analysis of different analytes in biological samples. Ethylenethiourea (ETU), a specific biotransformation product of ethylenebisdithiocarbamates (EBDCs), has antithyroid activity. Thus, the aim of this study was to optimize for the first time the DPX extraction technique for quantification of ETU in urine through gas chromatography mass spectrometry (GC/MS), validate, and apply this methodology. The DPX parameters were evaluated with univariate analysis: sorption phases, sample pH, sample volumes, cleaning, and elution solvents. This methodology can be considered environmentally friendly; therefore, it complies with the principles of Green Chemistry, using low volumes of solvents, thus generating few chemical residues during the analyses. The DPX/GC–MS method developed showed linearity for concentrations ranging from 100 to 1000&#xa0;µg L<sup>−1</sup>, with the coefficient of correlation (<i>r</i>) greater than 0.997 and the lack-of-fit test (<i>p </i>value) of 0.568 (<i>p</i> &gt; 0.05), and the LOQ was 100&#xa0;µg L<sup>−1</sup>. The intra-assay and inter-assay precision and accuracy showed acceptable values. Carryover was not observed according to acceptance criterion. It was found that there was a matrix effect (<i>p</i> &lt; 0.001) (rotational type), which was solved using an external standard of ETU in water and in the urine biological matrix. Most were collected after 24&#xa0;h of exposure to EBDCs, and the mean level of ETU was 4.07&#xa0;µg&#xa0;g<sup>−1</sup> creatinine. The DPX/GC–MS development method proved to be suitable for extraction and quantification of ETU in biological urine samples.</p>

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Disposable pipette extraction (DPX) of ethylenethiourea and analysis by gas chromatography coupled to mass spectrometry in urine samples of vineyard farmers

  • 期刊论文

  • 发表日期：

    2025年8月20日

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  • Jéssica Cristina Zoratto Romoli,
  • Deborah Thais Palma Scanferla,
  • Raul Gomes Aguera,
  • Renata Sano Lini,
  • Giseli Cristina Pante,
  • Carlos Roberto Bueno Jr.,
  • Juliana Cristina Castro,
  • Simone Aparecida Galerani Mossini,
  • Camila Marchioni,
  • Miguel Machinski Jr.

摘要

Disposable pipette extraction (DPX) is a modern miniaturized solid phase extraction technique that can be applied for analysis of different analytes in biological samples. Ethylenethiourea (ETU), a specific biotransformation product of ethylenebisdithiocarbamates (EBDCs), has antithyroid activity. Thus, the aim of this study was to optimize for the first time the DPX extraction technique for quantification of ETU in urine through gas chromatography mass spectrometry (GC/MS), validate, and apply this methodology. The DPX parameters were evaluated with univariate analysis: sorption phases, sample pH, sample volumes, cleaning, and elution solvents. This methodology can be considered environmentally friendly; therefore, it complies with the principles of Green Chemistry, using low volumes of solvents, thus generating few chemical residues during the analyses. The DPX/GC–MS method developed showed linearity for concentrations ranging from 100 to 1000 µg L−1, with the coefficient of correlation (r) greater than 0.997 and the lack-of-fit test (p value) of 0.568 (p > 0.05), and the LOQ was 100 µg L−1. The intra-assay and inter-assay precision and accuracy showed acceptable values. Carryover was not observed according to acceptance criterion. It was found that there was a matrix effect (p < 0.001) (rotational type), which was solved using an external standard of ETU in water and in the urine biological matrix. Most were collected after 24 h of exposure to EBDCs, and the mean level of ETU was 4.07 µg g−1 creatinine. The DPX/GC–MS development method proved to be suitable for extraction and quantification of ETU in biological urine samples.