Development of a simple analytical method for the simultaneous determination of paracetamol, paracetamol-glucuronide and p-aminophenol in river water

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2013-07, Vol.930, p.75-81
• Main Authors: Santos, Lúcia H.M.L.M., Paíga, Paula, Araújo, Alberto N., Pena, Angelina, Delerue-Matos, Cristina, Montenegro, M. Conceição B.S.M.
• Format: Article
• Language: English
• Subjects: acetaminophen; Acetaminophen - analogs & derivatives; Acetaminophen - analysis; Acetaminophen - chemistry; Acetaminophen - isolation & purification; adsorbents; Aminophenols - analysis; Aminophenols - chemistry; Aminophenols - isolation & purification; Arrays; Cartridges; Chromatography, High Pressure Liquid - methods; detection limit; Economic conditions; High performance liquid chromatography; HPLC; Limit of Detection; Linear Models; Mathematical analysis; Metabolites; p-Aminophenol; Paracetamol; Paracetamol-glucuronide; Portugal; Reproducibility of Results; River water; Rivers; Rivers - chemistry; Solid phase extraction; Solid Phase Extraction - methods; Transformations; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - chemistry; Water Pollutants, Chemical - isolation & purification
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2013.04.032

•Determination of paracetamol, paracetamol-glucuronide and p-aminophenol in rivers.•Development of a SPE procedure for their simultaneous determination.•All compounds were detected in rivers with concentrations up to few μg/L.•First time that paracetamol-glucuronide was found in river water. 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.