数字农科院2.0

Dual SPE-UPLC-MS/MS method for multi-residue determination of anthelmintics in bovine tissues

文献类型： 外文期刊

作者： Guonian Dai;Yaxin Zhou;Bintao Zhai;Haiquan Li;Yuyin Dai;Qing Wang;Xuzheng Zhou;Jiyu Zhang

作者机构：

关键词： Compound Oxyclozanide suspension;MRLs;Multi-residue determination;Tissue distribution;UPLC-MS/MS;Veterinary drug residues;Withdrawal period

期刊名称： Microchemical Journal

ISSN： 0026-265X

年卷期： 2025 年 216 卷

页码：

收录情况： SCIE（2025版）

摘要： This study establishes a sensitive Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS) method for multi-residue determination of Compound Oxyclozanide Suspension components in bovine tissues using 20 Simmental cattle (10 males, 10 females). A novel dual extraction-purification protocol addressed veterinary drug monitoring challenges: Oxyclozanide (OXY) and Niclosamide (NIC) were isolated via acetonitrile-acetone (6:4) liquid-liquid extraction with CNWBOND MAX SPE cleanup, while Levamisole Hydrochloride (LEV) and Mebendazole (MED) required ethyl acetate extraction followed by Oasis MCX SPE purification. Validated across liver, kidney, muscle, and fat matrices, the method achieved recoveries of 84.13–106.45 % with intra−/inter-day precision (RSDs <12.55 %) at quantification ranges of 2.5–1250 μg/kg (OXY) and 2.5–220 μg/kg (LEV). Residue kinetics revealed peak tissue concentrations of 11,560 μg/kg (OXY) and 6452 μg/kg (LEV) in liver, followed by 8983 μg/kg (OXY) and 6201 μg/kg (LEV) in kidney, with significantly lower levels in muscle (720.10 μg/kg OXY; 1685 μg/kg LEV) and fat (277.40 μg/kg OXY; 377.10 μg/kg LEV). Critical depletion analysis confirmed final residues in all tissues fell below EU and China maximum residue limits (MRLs) at calculated withdrawal periods. Tissue-specific intervals were determined as 23.72 days (liver), 22.00 days (kidney), 20.80 days (muscle), and 24.82 days (fat) for OXY, and 18.72, 26.25, 27.86, and 21.35 days for LEV, respectively. To ensure international regulatory compliance, a harmonized 28-day withdrawal period is proposed based on the most conservative tissue-specific data. This work establishes pivotal pharmacokinetic benchmarks and validates a sensitive multi-residue analytical framework, significantly advancing the science-based application of Compound Oxyclozanide Suspension in veterinary therapeutics.

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