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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： Dai, Guonian 1 ; Zhou, Yaxin 1 ; Zhai, Bintao 1 ; Li, Haiquan 1 ; Dai, Yuyin 1 ; Wang, Qing 1 ; Zhou, Xuzheng 1 ; Zhang, Jiyu 1 ;

作者机构： 1.Chinese Acad Agr Sci, Lanzhou Inst Husb & Pharm Ceut Sci, Key Lab Vet Pharmaceut Dev, Minist Agr & Rural Affairs, Lanzhou 730050, Peoples R China

2.Gansu Agr Univ, Coll Vet Med, Lanzhou 730070, Peoples R China

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

期刊名称：MICROCHEMICAL JOURNAL （ 影响因子：5.1； 五年影响因子：4.7 ）

ISSN： 0026-265X

年卷期： 2025 年 216 卷

页码：

收录情况： SCI

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 g/kg (OXY) and 2.5-220 mu g/kg (LEV). Residue kinetics revealed peak tissue concentrations of 11,560 mu g/kg (OXY) and 6452 mu g/kg (LEV) in liver, followed by 8983 mu g/kg (OXY) and 6201 mu g/kg (LEV) in kidney, with significantly lower levels in muscle (720.10 mu g/kg OXY; 1685 mu g/kg LEV) and fat (277.40 mu g/kg OXY; 377.10 mu g/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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