Celano Rita, Piccinelli Anna Lisa, Campone Luca, Rastrelli Luca
Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy.
Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy.
J Chromatogr A. 2014 Aug 15;1355:26-35. doi: 10.1016/j.chroma.2014.06.009. Epub 2014 Jun 7.
Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD <10%) and very high enrichment factors were attained for different aqueous matrices (drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments.
药品和个人护理产品（PPCPs）是最重要的一类新兴污染物。与PPCPs相关的生态和环境影响潜力尤其令人担忧，因为它们不断渗透到水环境中。这项工作描述了一种新型的超预浓缩技术，用于对环境水基质中ppt水平的选定PPCPs进行快速且高灵敏度分析。通过固相萃取结合分散液液微萃取（SPE-DLLME）从大量水溶液（500和250mL）中快速提取并浓缩选定的PPCPs，然后使用超高效液相色谱-串联质谱（UHPLC-MS/MS）进行分析。仔细研究并优化了实验参数，以实现最佳的SPE-DLLME效率和更高的富集因子。使用乙腈/甲醇/二氯甲烷3:3:4（v/v/v）的三元混合物作为SPE洗脱剂和DLLME萃取剂/分散混合物可获得最佳结果。还对DLLME水溶液（5% NaCl，10mgL⁻¹ 四丁基溴化铵）进行了改性，以提高更多亲水性PPCPs的萃取效率。在最佳条件下，对于大多数被研究的分析物实现了完全萃取（回收率>70%），不同水基质（饮用水、海水、河水和废水）的精密度（RSD<10%）和非常高的富集因子。对于15种选定的PPCPs，方法检测限和定量限分别处于非常低的ppt水平且低于1和3ngL⁻¹。所提出的分析程序具有许多优点，如操作简单、快速、富集因子高和灵敏度高。因此，它适用于监测和研究不同环境介质中PPCPs的存在情况。
