KWR Watercycle Research Institute, P.O. Box 1072, 3430 BB Nieuwegein, The Netherlands; Mass Spectrometry Laboratory, Chemistry Department, University of Liège, 4000 Liège, Belgium.
KWR Watercycle Research Institute, P.O. Box 1072, 3430 BB Nieuwegein, The Netherlands; Vitens N.V. Drinking Water Company, 8019BE Zwolle, The Netherlands.
Talanta. 2018 Aug 15;186:527-537. doi: 10.1016/j.talanta.2018.04.058. Epub 2018 Apr 27.
A novel sample preparation procedure relying on Solid Phase Extraction (SPE) combining different sorbent materials on a sequential-based cartridge was optimized and validated for the enrichment of 117 widely diverse contaminants of emerging concern (CECs) from surface waters (SW) and further combined chemical and biological analysis on subsequent extracts. A liquid chromatography coupled to high resolution tandem mass spectrometry LC-(HR)MS/MS protocol was optimized and validated for the quantitative analysis of organic CECs in SW extracts. A battery of in vitro CALUX bioassays for the assessment of endocrine, metabolic and genotoxic interference and oxidative stress were performed on the same SW extracts. Satisfactory recoveries ([70-130]%) and precision (< 30%) were obtained for the majority of compounds tested. Internal standard calibration curves used for quantification of CECs, achieved the linearity criteria (r > 0.99) over three orders of magnitude. Instrumental limits of detection and method limits of quantification were of [1-96] pg injected and [0.1-58] ng/L, respectively; while corresponding intra-day and inter-day precision did not exceed 11% and 20%. The developed procedure was successfully applied for the combined chemical and toxicological assessment of SW intended for drinking water supply. Levels of compounds varied from < 10 ng/L to < 500 ng/L. Endocrine (i.e. estrogenic and anti-androgenic) and metabolic interference responses were observed. Given the demonstrated reliability of the validated sample preparation method, the authors propose its integration in an effect-directed analysis procedure for a proper evaluation of SW quality and hazard assessment of CECs.
一种新颖的样品制备方法，依赖于固相萃取（SPE），将不同的吸附材料组合在基于顺序的小柱上，用于从地表水中富集 117 种广泛存在的新兴关注污染物（CECs），并进一步对后续提取物进行化学和生物分析。优化并验证了一种液相色谱与高分辨串联质谱联用（LC-（HR）MS/MS）方案，用于定量分析地表水中有机 CECs 的提取液。对同一地表水中的提取物进行了一系列体外 CALUX 生物测定，以评估内分泌干扰、代谢干扰、遗传毒性和氧化应激。对于大多数测试的化合物，都获得了令人满意的回收率（[70-130]%）和精密度（<30%）。用于定量 CECs 的内标校准曲线在三个数量级上达到了线性标准（r > 0.99）。仪器检测限和方法定量限分别为[1-96] pg 进样和[0.1-58] ng/L；而相应的日内和日间精密度不超过 11%和 20%。该方法成功地应用于饮用水源地表水的化学和毒理学综合评估。化合物的浓度从<10 ng/L 到<500 ng/L 不等。观察到了内分泌（即雌激素和抗雄激素）和代谢干扰的反应。鉴于所验证的样品制备方法的可靠性，作者建议将其整合到效应导向分析程序中，以正确评估地表水的质量和 CECs 的危害评估。
