title: Development of a simple analytical method for the simultaneous determination of paracetamol, paracetamol-glucuronide and p-aminophenol in river water.
abstract: Paracetamol is among the most worldwide consumed pharmaceuticals. Although its occurrence in the environment is well documented, data about the presence of its metabolites and transformation products is very scarce. The present work describes the development of an analytical method for the simultaneous determination of paracetamol, its principal metabolite (paracetamol-glucuronide) and its main transformation product (p-aminophenol) based on solid phase extraction (SPE) and high performance liquid chromatography coupled to diode array detection (HPLC-DAD). The method was applied to analysis of river waters, showing to be suitable to be used in routine analysis. Different SPE sorbents were compared and the use of two Oasis WAX cartridges in tandem proved to be the most adequate approach for sample clean up and pre-concentration. Under optimized conditions, limits of detection in the range 40-67ng/L were obtained, as well as mean recoveries between 60 and 110% with relative standard deviations (RSD) below 6%. Finally, the developed SPE-HPLC/DAD method was successfully applied to the analysis of the selected compounds in samples from seven rivers located in the north of Portugal. Nevertheless all the compounds were detected, it was the first time that paracetamol-glucuronide was found in river water at concentrations up to 3.57μg/L.
authors.affiliation: REQUIMTE, Faculty of Pharmacy, University of Porto, Rua Jorge Viterbo Ferreira 228, 4050-313 Porto, Portugal.
authors.forename: Lúcia H M L M
authors.initials: LH
authors.lastname: Santos
authors.forename: Paula
authors.initials: P
authors.lastname: Paíga
authors.forename: Alberto N
authors.initials: AN
authors.lastname: Araújo
authors.forename: Angelina
authors.initials: A
authors.lastname: Pena
authors.forename: Cristina
authors.initials: C
authors.lastname: Delerue-Matos
authors.forename: M Conceição B S M
authors.initials: MC
authors.lastname: Montenegro
mesh_terms: D000082:Acetaminophen / Q000031:analogs & derivatives* / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D000627:Aminophenols / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D057230:Limit of Detection; D016014:Linear Models; D011174:Portugal; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D000627:Aminophenols; D014874:Water Pollutants, Chemical; D000082:Acetaminophen; C037386:acetaminophen glucuronide; C026729:4-aminophenol