Research Group Environmental Organic Chemistry and Technology (EnVOC), Department of Sustainable Organic Chemistry and Technology, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent, Belgium.
Research Group Environmental Organic Chemistry and Technology (EnVOC), Department of Sustainable Organic Chemistry and Technology, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent, Belgium.
J Hazard Mater. 2017 Feb 5;323(Pt A):2-10. doi: 10.1016/j.jhazmat.2016.05.077. Epub 2016 May 27.
This research addresses some critical challenges regarding the validation of a quantitative multi-residue method for pharmaceuticals in wastewater making use of modern SPE-LC-Orbitrap high-resolution mass spectrometry. Particular attention is given to study in detail response linearity, to realistically estimate detection limits, and to express the measurement precision of the analyte concentration, obtained by external calibration. First, linearity of the Orbitrap response showed to be matrix dependent in a counter intuitive way: stronger deviations from linearity were observed for pure solvent standards than for complex matrices like wastewater. Second, detection limits risk to be overestimated for ubiquitously present compounds for which true blank matrix samples are hard to find, leading to false negative findings. A novel and easy applicable methodology is presented to allow a better estimation of detection limits using the response of the natural isotopes. Third, a statistical methodology to estimate the measurement precision of the analyte concentration using basic validation parameters is developed specifically for the context of multi-residue quantification.
本研究针对利用现代 SPE-LC-Orbitrap 高分辨率质谱法验证废水中药物的定量多残留方法的一些关键挑战进行了探讨。特别关注详细研究响应线性度，以实际估计检测限，并表达通过外部校准获得的分析物浓度的测量精密度。首先，Orbitrap 响应的线性度呈现出一种反直觉的基质依赖性：与复杂基质（如废水）相比，纯溶剂标准的线性偏差更大。其次，对于普遍存在的化合物，检测限存在被高估的风险，因为很难找到真正的空白基质样品，从而导致假阴性结果。提出了一种新颖且易于应用的方法，利用天然同位素的响应来更好地估计检测限。第三，专门针对多残留定量的情况，开发了一种使用基本验证参数估计分析物浓度测量精密度的统计方法。
