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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry
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Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry

机译：超高效液相色谱-串联质谱法对环境和废水样品中的约50种药物（包括26种抗生素）进行多类测定

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A multi-class method for the simultaneous quantification and confirmation of 47 pharmaceuticals in environmental and wastewater samples has been developed. The target list of analytes included analgesic and anti-inflammatories, cholesterol lowering statin drugs and lipid regulators, antidepressants, anti-ulcer agents, psychiatric drugs, ansiolitics, cardiovasculars and a high number (26) of antibiotics from different chemical groups. A common pre-concentration step based on solid-phase extraction with Oasis HLB cartridges was applied, followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) measurement. All compounds were satisfactorily determined in just one single injection, with a chromatographic run time of only 10. min. The process efficiency (combination of the matrix effect and the extraction process recovery) for the 47 selected compounds was evaluated in nine effluent wastewater (EWW) samples, and the use of different isotope-labelled internal standards (ILIS) was investigated to correct unsatisfactory values. Up to 12 ILIS were evaluated in EWW and surface water (SW). As expected, the ILIS provided satisfactory correction for their own analytes. However, the use of these ILIS for the rest of pharmaceuticals was problematic in some cases. Despite this fact, the correction with analogues ILIS was found useful for most of analytes in EWW, while was not strictly required in the SW tested. The method was successfully validated in SW and EWW at low concentration levels, as expected for pharmaceuticals in these matrices (0.025, 0.1 and 0.5 μg/L in SW; 0.1 and 0.5 μg/L in EWW). With only a few exceptions, the instrumental limits of detection varied between 0.1 and 8. pg. The limits of quantification were estimated from sample chromatograms at the lowest spiked levels tested and normally were below 20. ng/L for SW and below 50. ng/L for EWW. The developed method was applied to the analysis of around forty water samples (river waters and effluent wastewaters) from the Spanish Mediterranean region. Almost all the pharmaceuticals selected in this work were detected, mainly in effluent wastewater. In both matrices, analgesics and anti-inflammatories, lipid regulators and quinolone antibiotics were the most detected groups.
机译：开发了一种同时定量和确认环境和废水样品中47种药物的多类方法。分析物的目标清单包括止痛药和消炎药，降胆固醇的他汀类药物和脂质调节剂，抗抑郁药，抗溃疡药，精神病药，麻醉药，心血管药和来自不同化学组的大量抗生素（26）。应用了常见的预浓缩步骤，该步骤基于使用Oasis HLB柱进行固相萃取的步骤，然后进行超高效液相色谱-串联质谱（UHPLC-MS / MS）测量。仅一次进样就可以令人满意地测定所有化合物，色谱运行时间仅为10分钟。在9种废水（EWW）样品中评估了47种选定化合物的工艺效率（基质效应与萃取工艺回收率的结合），并研究了使用不同同位素标记的内标（ILIS）来纠正不满意的值。在EWW和地表水（SW）中评估了多达12种ILIS。正如预期的那样，ILIS为他们自己的分析物提供了令人满意的校正。但是，在某些情况下，将这些ILIS用于其余药品是有问题的。尽管如此，发现用类似物ILIS进行校正对于EWW中的大多数分析物还是有用的，而在测试的软件中并非严格要求。如在这些基质中的药物所期望的那样（在SW中为0.025、0.1和0.5μg/ L;在EWW中为0.1和0.5μg/ L），该方法已在SW和EWW中以低浓度水平成功验证。除少数例外，仪器的检测限在0.1至8 pg之间变化。定量限是从测试的最低加标水平下的样品色谱图估算得出的，SW低于20 ng / L，EWW低于50. ng / L。所开发的方法用于分析来自西班牙地中海地区的大约40个水样（河流水和废水）。几乎所有在这项工作中选择的药物都被检测到，主要是在废水中。在止痛药和消炎药这两种基质中，脂类调节剂和喹诺酮类抗生素含量最高。

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