Ens Waldemar, Senner Frank, Gygax Benjamin, Schlotterbeck Götz
Industrielle Werke Basel, Margarethenstrasse 40, 4002, Basel, Switzerland.
Anal Bioanal Chem. 2014 May;406(12):2789-98. doi: 10.1007/s00216-014-7712-0. Epub 2014 Mar 4.
A new method for the simultaneous determination of iodated X-ray contrast media (ICM) and artificial sweeteners (AS) by liquid chromatography-tandem mass spectrometry (LC-MS/MS) operated in positive and negative ionization switching mode was developed. The method was validated for surface, ground, and drinking water samples. In order to gain higher sensitivities, a 10-fold sample enrichment step using a Genevac EZ-2 plus centrifugal vacuum evaporator that provided excellent recoveries (90 ± 6 %) was selected for sample preparation. Limits of quantification below 10 ng/L were obtained for all compounds. Furthermore, sample preparation recoveries and matrix effects were investigated thoroughly for all matrix types. Considerable matrix effects were observed in surface water and could be compensated by the use of four stable isotope-labeled internal standards. Due to their persistence, fractions of diatrizoic acid, iopamidol, and acesulfame could pass the whole drinking water production process and were observed also in drinking water. To monitor the fate and occurrence of these compounds, the validated method was applied to samples from different stages of the drinking water production process of the Industrial Works of Basel (IWB). Diatrizoic acid was found as the most persistent compound which was eliminated by just 40 % during the whole drinking water treatment process, followed by iopamidol (80 % elimination) and acesulfame (85 % elimination). All other compounds were completely restrained and/or degraded by the soil and thus were not detected in groundwater. Additionally, a direct injection method without sample preparation achieving 3-20 ng/L limits of quantification was compared to the developed method.
开发了一种通过液相色谱-串联质谱法（LC-MS/MS）在正离子和负离子切换模式下同时测定碘化X射线造影剂（ICM）和人工甜味剂（AS）的新方法。该方法已针对地表水、地下水和饮用水样品进行了验证。为了获得更高的灵敏度，选择使用Genevac EZ-2 plus离心真空蒸发器进行10倍样品富集步骤，该步骤提供了出色的回收率（90±6%）用于样品制备。所有化合物的定量限均低于10 ng/L。此外，还对所有基质类型的样品制备回收率和基质效应进行了深入研究。在地表水中观察到了相当大的基质效应，可以通过使用四种稳定同位素标记的内标来补偿。由于它们的持久性，泛影酸、碘帕醇和安赛蜜的部分成分可以通过整个饮用水生产过程，在饮用水中也有发现。为了监测这些化合物的去向和存在情况，将经过验证的方法应用于巴塞尔工业厂（IWB）饮用水生产过程不同阶段的样品。发现泛影酸是最持久的化合物，在整个饮用水处理过程中仅被去除40%，其次是碘帕醇（80%去除）和安赛蜜（85%去除）。所有其他化合物被土壤完全截留和/或降解，因此在地下水中未被检测到。此外，还将一种无需样品制备的直接进样方法（定量限为3-20 ng/L）与所开发的方法进行了比较。
