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<p>The use of 5-nitroimidazoles such as metronidazole, dimetridazole, ronidazole, tinidazole, and ipronidazole against Nosema infections has raised significant health concerns because of their mutagenic and carcinogenic effects. Hence, their detection is highly important for precise and reliable food safety monitoring. This research optimized two extraction methods for 5-nitroimidazoles in honey, namely, 52734-U-SupelMIP™ solid-phase extraction and QuEChERS salt extraction, which were analysed via liquid chromatography-tandem mass spectrometry (LC‒MS/MS). The optimized method achieved detection limits of 0.05–0.19&#xa0;µg/kg and quantification limits of 0.33–0.46&#xa0;µg/kg. Linearity was demonstrated over the concentration range of 0.3–3.0&#xa0;µg/kg (R<sup>2</sup> &gt; 0.99), with repeatability below 17.24%, and RSD (%) and recovery rates ranging from 69.98% to 102.70%. 52734-U-SupelMIP™ solid-phase extraction showed 35.35% higher extraction efficiency than the QuEChERS salt extraction method. Analysis of 24 Albanian honey samples revealed nitroimidazole residues in 12.5% of the samples ([0.59–53.00&#xa0;µg/kg] range). Three samples exceeded the Commission Implementing Regulation (EU) 2021/808 minimum required performance limit (MRPL) of 1&#xa0;µg/kg, reaching up to 53.0&#xa0;µg/kg for metronidazole, underscoring the need for strict monitoring. This study delivers the first optimized comparison of SupelMIP™ columns, confirming their superior performance and importance for food safety.</p>

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Comparative study of 52734-U-SupelMIP™ solid-phase and QuEChERS extraction methods for monitoring 5-nitroimidazoles in Albanian honey

  • 期刊论文

  • 发表日期：

    2026年1月5日

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  • Kozeta Vaso,
  • Ina Pasho,
  • Landi Dardha,
  • Esenina Stroka

摘要

The use of 5-nitroimidazoles such as metronidazole, dimetridazole, ronidazole, tinidazole, and ipronidazole against Nosema infections has raised significant health concerns because of their mutagenic and carcinogenic effects. Hence, their detection is highly important for precise and reliable food safety monitoring. This research optimized two extraction methods for 5-nitroimidazoles in honey, namely, 52734-U-SupelMIP™ solid-phase extraction and QuEChERS salt extraction, which were analysed via liquid chromatography-tandem mass spectrometry (LC‒MS/MS). The optimized method achieved detection limits of 0.05–0.19 µg/kg and quantification limits of 0.33–0.46 µg/kg. Linearity was demonstrated over the concentration range of 0.3–3.0 µg/kg (R2 > 0.99), with repeatability below 17.24%, and RSD (%) and recovery rates ranging from 69.98% to 102.70%. 52734-U-SupelMIP™ solid-phase extraction showed 35.35% higher extraction efficiency than the QuEChERS salt extraction method. Analysis of 24 Albanian honey samples revealed nitroimidazole residues in 12.5% of the samples ([0.59–53.00 µg/kg] range). Three samples exceeded the Commission Implementing Regulation (EU) 2021/808 minimum required performance limit (MRPL) of 1 µg/kg, reaching up to 53.0 µg/kg for metronidazole, underscoring the need for strict monitoring. This study delivers the first optimized comparison of SupelMIP™ columns, confirming their superior performance and importance for food safety.