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首页> 外文期刊>Journal of mass spectrometry: JMS >Importance of MS selectivity and chromatographic separation in LC-MS/MS-based methods when investigating pharmaceutical metabolites in water. Dipyrone as a case of study
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Importance of MS selectivity and chromatographic separation in LC-MS/MS-based methods when investigating pharmaceutical metabolites in water. Dipyrone as a case of study

机译：在研究水中的药物代谢物时，基于LC-MS / MS的方法中MS选择性和色谱分离的重要性。双吡喃酮作为研究案例

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摘要

Pharmaceuticals are emerging contaminants of increasing concern because of their presence in the aquatic environment and potential to reach drinking-water sources. After human and/or veterinary consumption, pharmaceuticals can be excreted in unchanged form, as the parent compound, and/or as free or conjugated metabolites. Determination of most pharmaceuticals and metabolites in the environment is commonly made by liquid chromatography (LC) coupled to mass spectrometry (MS). LC coupled to tandem MS is the technique of choice nowadays in this field. The acquisition of two selected reaction monitoring (SRM) transitions together with the retention time is the most widely accepted criterion for a safe quantification and confirmation assay. However, scarce attention is normally paid to the selectivity of the selected transitions as well as to the chromatographic separation. In this work, the importance of full spectrum acquisition high-resolution MS data using a hybrid quadrupole time-of-flight analyser and/or a suitable chromatographic separation (to reduce the possibility of co-eluting interferences) is highlighted when investigating pharmaceutical metabolites that share common fragment ions. For this purpose, the analytical challenge associated to the determination of metabolites of the widely used analgesic dipyrone (also known as metamizol) in urban wastewater is discussed. Examples are given on the possibilities of reporting false positives of dypirone metabolites by LC-MS/MS under SRM mode due to a wrong assignment of identity of the compounds detected.
机译：由于药物在水生环境中的存在以及潜在的饮用水来源，因此它们正成为人们日益关注的新兴污染物。人和/或兽医食用后，药物可以母体化合物形式和/或游离或结合的代谢物形式不变地排泄。环境中大多数药物和代谢物的测定通常是通过液相色谱（LC）结合质谱（MS）进行的。液相色谱与串联质谱联用是当今该领域的首选技术。获得两个选定的反应监测（SRM）离子对以及保留时间是安全定量和确认分析最广泛接受的标准。但是，通常很少注意所选过渡的选择性以及色谱分离。在这项工作中，在研究药物代谢物时，强调了使用混合四极杆飞行时间分析仪和/或适当的色谱分离（以减少共洗脱干扰的可能性）全光谱采集高分辨率MS数据的重要性。共享共同的碎片离子。为此，讨论了与测定城市废水中广泛使用的止痛双嘧啶（也称为metmizol）的代谢物有关的分析挑战。给出了有关由于检测到的化合物的身份分配不正确而在SRM模式下通过LC-MS / MS报告Dypirone代谢物假阳性的可能性的示例。

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