Confirmation of 13 sulfonamides in honey by liquid chromatography-tandem mass spectrometry for monitoring plans: Validation according to European Union Decision 2002/657/EC
Confirmation of 13 sulfonamides in honey by liquid chromatography-tandem mass spectrometry for monitoring plans: Validation according to European Union Decision 2002/657/EC
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DOI：
10.1016/j.chroma.2014.03.003
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发表时间：
2014-04-25
影响因子：
4.1
通讯作者：
Hurtaud-Pessel, Dominique
中科院分区：
文献类型：
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作者：
Dubreil-Cheneau, Estelle;Pirotais, Yvette;Hurtaud-Pessel, Dominique
根据欧盟委员会第 2002/657/EC 号决定，开发了一种快速可靠的液相色谱-串联质谱 (LC-MS/MS) 方法，用于同时确认蜂蜜中的 13 种磺胺类药物，并进行了充分验证。验证方案是按照所有分析物50 mu g kg(-1) 的目标水平构建的。研究的磺胺类药物如下：磺胺胍（SGN）、磺胺（SNL）、磺胺嘧啶（SDZ）、磺胺噻唑（STZ）、磺胺甲基嘧啶（SMR）、磺胺二甲唑（SMZ）、磺胺二甲嗪（SDM）、磺胺间甲氧嘧啶（SMNM）、磺胺甲氧基哌达嗪（SMP）、磺胺多辛(SDX)、磺胺甲恶唑 (SMX)、磺胺喹喔啉 (SQX) 和磺胺二甲氧嘧啶 (SOT)。在开发阶段研究了几种提取程序。最后，通过使用酸性水解和阳离子交换纯化的程序获得了最好的结果。在C18分析柱上实现色谱分离。还研究了基质效应。通过在正电喷雾模式下监测每个分析物的 2 个 MRM 转换来执行用于验证目的的数据采集。在实验室内重现性条件下，平均相对回收率范围为 85.8% 至 110.2%，相对标准偏差范围为 2.6% 至 19.8%。决策限(CC alpha)范围为1.8至15.5μg·kg(-1)。使用高分辨率质谱法研究蜂蜜中磺酰胺代谢物的可能形成。验证结果证明该方法适用于法国蜜蜂磺胺类药物残留监测计划实施的筛选和确证步骤。 (C) 2014 Elsevier B.V. 保留所有权利。
A rapid and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous confirmation of 13 sulfonamides in honey was developed and fully validated in accordance with the European Commission Decision No 2002/657/EC. The validation scheme was built in accordance with the target level of 50 mu g kg(-1) for all analytes. The sulfonamides investigated were as follows: sulfaguanidine (SGN), sulfanilamide (SNL), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethizole (SMZ), sulfadimerazine (SDM), sulfamonomethoxine (SMNM), sulfamethoxypiridazine (SMP), sulfadoxine (SDX), sulfamethoxazole (SMX), sulfaquinoxaline (SQX) and sulfadimethoxine (SOT). Several extraction procedures were investigated during the development phase. Finally, the best results were obtained with a procedure using acidic hydrolysis and cation exchange purification. Chromatographic separation was achieved on a C18 analytical column. Matrix effects were also investigated. Data acquisition implemented for the confirmatory purpose was performed by monitoring 2 MRM transitions per analyte under the positive electrospray mode. Mean relative recoveries ranged from 85.8% to 110.2% and relative standard deviations lying between 2.6% and 19.8% in intra-laboratory reproducibility conditions. The decision limits (CC alpha) ranged from 1.8 to 15.5 mu g kg(-1). High resolution mass spectrometry was used to investigate the possible formation of sulfonamide metabolites in honey. The validation results proved that the method is suitable for the screening and confirmatory steps as implemented for the French monitoring residue plan for sulfonamides residue control in honeybees. (C) 2014 Elsevier B.V. All rights reserved.