Analysis of 76 veterinary pharmaceuticals from 13 classes including aminoglycosides in bovine muscle by hydrophilic interaction liquid chromatography-tandem mass spectrometry
Analysis of 76 veterinary pharmaceuticals from 13 classes including aminoglycosides in bovine muscle by hydrophilic interaction liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.chroma.2016.05.031
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发表时间：
2016-06-24
影响因子：
4.1
通讯作者：
Thomaidis, Nikolaos S.
中科院分区：
文献类型：
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作者：
Dasenaki, Marilena E.;Michali, Christina S.;Thomaidis, Nikolaos S.
根据欧盟委员会决定 2002/657/EC 的要求，开发并验证了一种同时测定牛肌肉组织中 76 种兽药和药物的多残留/多类方法。这些分析物属于 13 个不同类别，其中包括氨基糖苷类抗生素，其不同的理化性质（极强的极性）使其与其他兽药的同时测定变得相当困难。该方法将两步萃取程序（用乙腈萃取，然后用酸性水缓冲液萃取）与亲水相互作用液相色谱-串联质谱 (HILIC-MS/MS) 测定相结合，从而可以在单次色谱运行中进行确认和定量。使用聚合物 SPE 柱通过固相萃取进行进一步净化。对氨基糖苷类进行了彻底的电离研究，以提高其灵敏度，并揭示了分析物前体离子丰度的显着差异，具体取决于测试流动相的组成。对所有目标分析物进行了进一步的梯度洗脱优化和进样溶剂优化。该方法根据欧盟委员会决定 2002/657 进行了验证。通过标准添加校准的方式进行定量分析。在最低验证水平下，回收率从 37.4%（溴己新）到 106%（卡那霉素）不等，82% 的化合物显示回收率 >70%。检测能力(CC beta)从2.4(盐霉素)到1302(安普霉素)μg kg(-1)不等。 (C) 2016 Elsevier B.V. 保留所有权利。
A multiresidue/multiclass method for the simultaneous determination of 76 veterinary drugs and pharmaceuticals in bovine muscle tissue has been developed and validated according to the requirements of European Commission Decision 2002/657/EC. The analytes belong in 13 different classes, including aminoglycoside antibiotics, whose different physicochemical properties (extremely polar character) render their simultaneous determination with other veterinary drugs quite problematic. The method combines a two-step extraction procedure (extraction with acetonitrile followed by an acidic aqueous buffer extraction) with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination, allowing confirmation and quantification in a single chromatographic run. Fulther cleanup with solid phase extraction was performed using polymeric SPE cartridges. A thorough ionization study of aminoglycosides was performed in order to increase their sensitivity and significant differences in the abundance of the precursor ions of the analytes were revealed, depending on the composition of the mobile phase tested. Further gradient elution optimization and injection solvent optimization were performed for all target analytes.The method was validated according to the European Commission Decision 2002/657. Quantitative analysis was performed by means of standard addition calibration. Recoveries varied from 37.4% (bromhexine) to 106% (kanamycin) in the lowest validation level and 82% of the compounds showed recovery >70%. Detection capability (CC beta) varied from 2.4 (salinomycin) to 1302 (apramycin) mu g kg(-1). (C) 2016 Elsevier B.V. All rights reserved.