Determination of nitrated and oxygenated polycyclic aromatic hydrocarbons in water samples by a liquid–liquid phase microextraction procedure based on the solidification of a floating organic drop followed by solvent assisted back-extraction and liquid chromatography–tandem mass spectrometry

GUIÑEZ, MARÍA; CERUTTI, SOLEDAD; MARTINEZ, LUIS D.; BAZAN, CRISTIAN; GUIÑEZ, MARÍA; CERUTTI, SOLEDAD; MARTINEZ, LUIS D.; BAZAN, CRISTIAN

MICROCHEMICAL JOURNAL

ELSEVIER SCIENCE BV

Año: 2018 vol. 139 p. 164 - 173

0026-265X

A methodology was optimized for the determination of nitrated-PAHs (nitro-PAHs) and oxygenated-PAHs (oxy-PAHs) in natural waters. The extraction/preconcentration procedure was performed by liquid?liquid phase microextraction based on the solidification of a floating organic drop followed by a novel solvent assisted back-extraction (DLLME-SFO-SBE) combined with liquid chromatography-tandem mass spectrometry. The solvent assisted back extraction into a suitable solvent enabled the direct injection of nitro and oxy-PAHs into the UHPLC-(+)APCI-MS/MS system. Parameters affecting the efficiency of the back-extraction procedure were evaluated and optimized, including the nature of the back-extractant volume, temperature and agitation effect. Additionally, various strategies related to the emulsion formation process were assayed.Detection and quantification limits were in the range of 0.02?0.85 ng mL−1 and 0.15?1.10 ng mL−1. Acceptable extraction recoveries between 95.1 and 100% and enrichment factors between 192 and 200-fold, with relative standard deviations