Determination of fourteen non-steroidal anti-inflammatory drugs in animal serum and plasma by liquid chromatography/mass spectrometry.
Determination of fourteen non-steroidal anti-inflammatory drugs in animal serum and plasma by liquid chromatography/mass spectrometry.
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DOI：
10.1002/rcm.2748
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发表时间：
2006-11
期刊：
影响因子：
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通讯作者：
F. Vinci;Serena Fabbrocino;M. Fiori;L. Serpe;P. Gallo
中科院分区：
文献类型：
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作者：
F. Vinci;Serena Fabbrocino;M. Fiori;L. Serpe;P. Gallo
欧盟规范了非甾体抗炎药（NSAIDs）在动物生产中的使用，并要求其成员国检测其在不同基质中的残留。在这项工作中，详细的MS和MS/MS离子阱质谱研究描述了14种非甾体抗炎药。建立了水杨酸、萘普生、卡洛芬、氟比洛芬、布洛芬、尼氟酸和甲氯芬酸的多残留反相LC/ESI-MS/MS检测方法，以及酮洛芬、苏西布他酮、双氯芬酸、甲非那酸、甲苯非那酸、苯丁酮及其代谢物氧苯丁酮的多残留反相LC/ESI-MS检测方法。因此，通过线性梯度色谱分离后，可以在养殖动物的血清和血浆样品中确认多达14种不同的非甾体抗炎药残留。这些物质被选为非甾体抗炎药不同化学亚类的代表。两种方法也在三种污染水平下进行了内部验证，评估特异性并计算平均回收率、重复性和实验室内再现性。质谱/质谱产物离子谱成功地对所测药物进行了定性鉴定。除水杨酸外，所有非甾体抗炎药的回收率均较高，在71.6% ~ 100.9%之间。
The European Union has regulated the use of non-steroidal anti-inflammatory drugs (NSAIDs) in animal production and requires its member states to detect their residues in different matrices. In this work, a detailed MS and MS/MS study by ion-trap mass spectrometry of fourteen NSAIDs is described. Two multi-residue reversed-phase LC/ESI-MS/MS methods were developed, one for the determination of salicylic acid, naproxen, carprofen, flurbiprofen, ibuprofen, niflumic acid and meclofenamic acid in the negative ion mode, and the other for the determination of ketoprofen, suxibutazone, diclofenac, mefenamic acid, tolfenamic acid, phenylbutazone and its metabolite oxyphenbutazone in the positive ion mode. It was thus possible to confirm up to 14 different NSAID residues in serum and plasma samples of farmed animals, after chromatographic separation by a linear gradient. These substances were chosen as representative of different chemical subclasses of NSAIDs. The two methods were also validated in-house at three contamination levels, evaluating specificity and calculating mean recoveries, repeatability and within-laboratory reproducibility. The MS/MS product ion spectra were successfully used for the qualitative identification of all the drugs tested. All the NSAIDs, apart from salicylic acid, were recovered in high amounts, ranging between 71.6% and 100.9%.