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<p>The use of pesticides in rice production and storage is common practice and residue analysis is of great importance. This study aimed to develop and validate a miniaturized and simplified sample preparation method based on the solid-phase matrix dispersion (MSPD) technique for the multiresidue determination of pesticide residues in rice by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). All sample preparation was carried out in a single tube, without the need for a mortar and pestle or transfer to a cartridge as is the case with the classic MSPD technique. This modification simplifies execution, reducing possible losses of analytes and minimizing the risk of cross-contamination. Several tests were conducted to optimize the extraction, including the evaluation of solvents, sorbent types and masses, use of ultrasound, and dilution solvents. The extraction used only 0.5&#xa0;g of sample and a material of natural origin, diatomaceous earth, as sorbent, followed by extraction with acetonitrile containing 1% (v/v) acetic acid in ultrasound. The method showed recoveries from 70 to 120%, and RSD ≤ 20% for most of the levels evaluated. The limits of quantification (LOQ) were from 4 to 8&#xa0;μg&#xa0;kg<sup>−1</sup> for the 60 validated compounds. Method application to commercial rice revealed the presence of pesticide residues from the LOQ to 446&#xa0;μg&#xa0;kg<sup>−1</sup>, highlighting the importance of monitoring for food safety. The results obtained were compared to QuEChERS acetate method by the Student’s <i>t</i> test showing high agreement, indicating that the proposed method is efficient and suitable for routine analysis.</p>

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Miniaturized Straightforward Matrix Solid-Phase Dispersion for Multiresidue Determination of Pesticide Residues in Rice by UHPLC-MS/MS

  • 期刊论文

  • 发表日期：

    2025年8月29日

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  • Igor Franceschi de Souza,
  • Dylan Mehler Hoffmann,
  • Luana Floriano,
  • Magali Kemmerich,
  • Osmar Damian Prestes,
  • Renato Zanella

摘要

The use of pesticides in rice production and storage is common practice and residue analysis is of great importance. This study aimed to develop and validate a miniaturized and simplified sample preparation method based on the solid-phase matrix dispersion (MSPD) technique for the multiresidue determination of pesticide residues in rice by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). All sample preparation was carried out in a single tube, without the need for a mortar and pestle or transfer to a cartridge as is the case with the classic MSPD technique. This modification simplifies execution, reducing possible losses of analytes and minimizing the risk of cross-contamination. Several tests were conducted to optimize the extraction, including the evaluation of solvents, sorbent types and masses, use of ultrasound, and dilution solvents. The extraction used only 0.5 g of sample and a material of natural origin, diatomaceous earth, as sorbent, followed by extraction with acetonitrile containing 1% (v/v) acetic acid in ultrasound. The method showed recoveries from 70 to 120%, and RSD ≤ 20% for most of the levels evaluated. The limits of quantification (LOQ) were from 4 to 8 μg kg−1 for the 60 validated compounds. Method application to commercial rice revealed the presence of pesticide residues from the LOQ to 446 μg kg−1, highlighting the importance of monitoring for food safety. The results obtained were compared to QuEChERS acetate method by the Student’s t test showing high agreement, indicating that the proposed method is efficient and suitable for routine analysis.