Multiresidue analytical method for the determination of antimicrobials, preservatives, benzotriazole UV stabilizers, flame retardants and plasticizers in fish using ultra high performance liquid chromatography coupled with tandem mass spectrometry

Abstract

A multiresidue analytical method for the determination of emerging pollutants belonging to personal care products (PCPs) (antimicrobials, preservatives), benzotriazole UV stabilizers (BUVSs) and organophosphorus compounds (OPCs) in fish has been developed using high speed solvent extraction (HSSE) followed by silica gel clean up and ultra fast liquid chromatography coupled with tandem mass spectrometry (UFLC-MS/MS) analysis. Developed extraction and clean up method yielded good recovery (> 70%) for all the four groups of emerging pollutants, i.e. antimicrobials (78.5-85.6%), preservatives (85.0-89.4%), BUVSs (70.9-112%) and OPCs (81.6-114%; except for TEP - 68.9% and TPeP - 58.1%) with RSDs ranging from 0.7 to 15.4%. Intra- and inter-day repeatabilities were less than 19.8% and 19.0%, respectively at three spiked levels. The concentrations were given in lipid weight (lw) basis, and the method detection limits were achieved in the lowest range of 0.001-0.006 ng g⁻¹ for two antimicrobials, 0.001-0.015 ng g⁻¹ for four preservatives, 0.0002-0.009 ng g⁻¹ for eight BUVSs and 0.001-0.014 ng g⁻¹ for nine OPCs. Finally, the method was successfully validated as a simple and fast extraction method for the determination of 23 compounds belonging to PCPs, BUVSs and OPCs and applied to the analysis of three species of fish from Manila Bay, the Philippines. Concentrations ranged from 27 to 278 ng g⁻¹ for antimicrobials, 6.61 to 1580 ng g⁻¹ for paraben preservatives, <MDL (method detection limit) to 179 ng g⁻¹ for BUVSs and ND (not detected) to 266 ng g⁻¹ for OPCs suggesting the ubiquitous contamination by these emerging pollutants in Manila Bay. This is the first method developed for the determination of triclocarban, four paraben preservatives and four BUVSs, in fish.