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<p>In this study, an integrated method combining simultaneous extraction with UHPLC‒MS/MS analysis was introduced to detect 24 veterinary drug residues, including penicillins, quinolones, tetracyclines and antiparasitics, in beef and mutton rumps. The samples were pretreated with 0.1% formic acid in acetonitrile and 0.1&#xa0;mol/L Na₂EDTA<b>‒</b>Mcllvaine buffer (pH = 5.0). For separation, a BEH C<sub>18</sub> column (2.1 × 100&#xa0;mm, 1.7&#xa0;μm) was used, utilizing a gradient elution program with 0.1% formic acid in water and a methanol<b>‒</b>acetonitrile mixture (2:8, v/v). The analysis was performed using multiple reaction monitoring mode, with the source operating in positive ion scanning mode. Method validation revealed that the ranges of recovery, limits of detection and quantitation, and relative standard deviations were 70.1%<b>‒</b>97.0%, 0.1–1.5&#xa0;μg/kg, 0.5–5&#xa0;μg/kg and 3.7%–12.0%, respectively, which meet the requirements for 24 veterinary drug residue screenings in China and the European Union. In the proposed method, high-throughput screening was integrated with accurate quantification, overcoming the limitations of some current high-throughput techniques that focus solely on qualitative analysis and do not provide sufficient quantitative capability. Analysis of real samples revealed that only 3 samples had target veterinary drug residues, all of which were significantly below the maximum residue limits.</p> Graphical Abstract <p></p>

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Development and Validation of a UHPLC‒MS/MS Method Coupled with Liquid‒liquid Extraction and Solid-phase Extraction for 24 Veterinary Drug Residues in Beef and Mutton Rumps

  • 期刊论文

  • 发表日期：

    2026年7月28日

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  • Yiwei Hong,
  • Yali Zhu,
  • Junjie Xu,
  • Yuhan Xu,
  • Pengfei Gao,
  • Hao Chen,
  • Xu Liu,
  • Yi Sun,
  • Maoda Pang,
  • Genxi Zhang,
  • Tao Zhang,
  • Xiaodong Guo,
  • Xing Xie,
  • Kaizhou Xie

摘要

In this study, an integrated method combining simultaneous extraction with UHPLC‒MS/MS analysis was introduced to detect 24 veterinary drug residues, including penicillins, quinolones, tetracyclines and antiparasitics, in beef and mutton rumps. The samples were pretreated with 0.1% formic acid in acetonitrile and 0.1 mol/L Na₂EDTA‒Mcllvaine buffer (pH = 5.0). For separation, a BEH C18 column (2.1 × 100 mm, 1.7 μm) was used, utilizing a gradient elution program with 0.1% formic acid in water and a methanol‒acetonitrile mixture (2:8, v/v). The analysis was performed using multiple reaction monitoring mode, with the source operating in positive ion scanning mode. Method validation revealed that the ranges of recovery, limits of detection and quantitation, and relative standard deviations were 70.1%‒97.0%, 0.1–1.5 μg/kg, 0.5–5 μg/kg and 3.7%–12.0%, respectively, which meet the requirements for 24 veterinary drug residue screenings in China and the European Union. In the proposed method, high-throughput screening was integrated with accurate quantification, overcoming the limitations of some current high-throughput techniques that focus solely on qualitative analysis and do not provide sufficient quantitative capability. Analysis of real samples revealed that only 3 samples had target veterinary drug residues, all of which were significantly below the maximum residue limits.

Graphical Abstract