title: Multi-residue method for determination of 58 pesticides, pharmaceuticals and personal care products in water using solvent demulsification dispersive liquid-liquid microextraction combined with liquid chromatography-tandem mass spectrometry.
abstract: A rapid and efficient sample pretreatment using solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was studied for the extraction of 58 pharmaceuticals and personal care products (PPCPs) and pesticides from water samples. Type and volume of extraction and disperser solvents, pH, salt addition, amount of salt and type of demulsification solvent were evaluated. Limits of quantification (LOQ) in the range from 0.0125 to 1.25 µg L(-1) were reached, and linearity was in the range from the LOQ of each compound to 25 μg L(-1). Recoveries ranged from 60% to 120% for 84% of the compounds, with relative standard deviations lower than 29%. The proposed method demonstrated, for the first time, that sample preparation by SD-DLLME with determination by LC-MS/MS can be successfully used for the simultaneous extraction of 32 pesticides and 26 PPCPs from water samples. The entire procedure, including the extraction of 58 organic compounds from the aqueous sample solution and the breaking up of the emulsion after extraction with water, rather than with an organic solvent, was environmentally friendly. In addition, this technique was less expensive and faster than traditional techniques. Finally, the analytical method under study was successfully applied to the analysis of all 58 pesticides and PPCPs in surface water samples.
authors.affiliation: Escola de Química e Alimentos, Universidade Federal do Rio Grande-FURG, 96203-900 Rio Grande, RS, Brazil.
authors.forename: Sergiane Souza
authors.initials: SS
authors.lastname: Caldas
authors.affiliation: Escola de Química e Alimentos, Universidade Federal do Rio Grande-FURG, 96203-900 Rio Grande, RS, Brazil.
authors.forename: Caroline
authors.initials: C
authors.lastname: Rombaldi
authors.affiliation: Escola de Química e Alimentos, Universidade Federal do Rio Grande-FURG, 96203-900 Rio Grande, RS, Brazil.
authors.forename: Jean Lucas de Oliveira
authors.initials: JL
authors.lastname: Arias
authors.affiliation: Escola de Química e Alimentos, Universidade Federal do Rio Grande-FURG, 96203-900 Rio Grande, RS, Brazil.
authors.forename: Liziane Cardoso
authors.initials: LC
authors.lastname: Marube
authors.affiliation: Escola de Química e Alimentos, Universidade Federal do Rio Grande-FURG, 96203-900 Rio Grande, RS, Brazil. Electronic address: eprimelfurg@gmail.com.
authors.forename: Ednei Gilberto
authors.initials: EG
authors.lastname: Primel
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D003358:Cosmetics / Q000032:analysis* / Q000302:isolation & purification; D004655:Emulsions; D006863:Hydrogen-Ion Concentration; D059627:Liquid Phase Microextraction / Q000379:methods*; D010575:Pesticides / Q000032:analysis* / Q000302:isolation & purification; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000302:isolation & purification; D012492:Salts / Q000737:chemistry; D012997:Solvents / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification
chemical_list: D003358:Cosmetics; D004655:Emulsions; D010575:Pesticides; D004364:Pharmaceutical Preparations; D012492:Salts; D012997:Solvents; D014874:Water Pollutants, Chemical; D014867:Water
keywords: Dispersive liquid–liquid microextraction; Liquid chromatography; Mass spectrometry; Personal care products; Pesticides; Pharmaceuticals; Water samples