title: Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.
abstract: 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.
authors.affiliation: Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy.
authors.forename: Rita
authors.initials: R
authors.lastname: Celano
authors.affiliation: Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy. Electronic address: apiccine@unisa.it.
authors.forename: Anna Lisa
authors.initials: AL
authors.lastname: Piccinelli
authors.affiliation: Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy.
authors.forename: Luca
authors.initials: L
authors.lastname: Campone
authors.affiliation: Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084 Fisciano, Salerno, Italy.
authors.forename: Luca
authors.initials: L
authors.lastname: Rastrelli
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D059627:Liquid Phase Microextraction / Q000379:methods*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis
chemical_list: D014874:Water Pollutants, Chemical; D014867:Water
keywords: Dispersive liquid liquid microextraction; Environmental water matrices; Pharmaceutical and personal care products; Solid phase extraction; UHPLC–MS/MS