Quantification of Diclofenac in Hospital Effluent and Identification of Metabolites and Degradation Products

• Published in: Clean : soil, air, water air, water, 2012-09, Vol.40 (9), p.950-957
• Main Authors: Minetto, Luciane, Mayer, Francieli M., Mallmann, Carlos A., Martins, Ayrton F.
• Format: Article
• Language: English
• Subjects: Ammonium; Degradation products; Effluents; Hospital wastes; LC-ESI-MS/MS_QTrap; Liquid chromatography; Medical wastes; Metabolites; Methanol; Microcontamination; Pharmaceutical residue; Photolysis; Wastewater treatment; Xenobiotic
• ISSN: 1863-0650; 1863-0669
• DOI: 10.1002/clen.201100676

In this study the occurrence of diclofenac and sub‐products in effluent emerging from the University Hospital at the Federal University of Santa Maria was investigated. One metabolite was identified and, in aqueous solution, three degradation products. The quantification was conducted by means of HPLC‐DAD, and the determination of metabolite and degradation products by LC–ESI–MS/MS–QTrap. For the HPLC‐DAD method, a 70:30 mixture of methanol/sodium phosphate was used in isocratic mode. For the LC–ESI–MS/MS–QTrap determinations, a mobile phase, where phase A was an ammonium acetate solution 5 × 10−3 mol L−1, and phase B was methanol (5 × 10−3 mol L−1)/ammonium acetate (9:1, v/v), on gradient mode. The LDs for the HPLC and LC–MS/MS methods, respectively, were 2.5 and 0.02 µg L−1, the LQs, 8.3 and 0.05 µg L−1, and the linear range from 10 up to 2000 µg L−1 and 0.05 up to 10 µg L−1. As expected, the LC–ESI–MS/MS–QTrap method was more sensitive and less laborious. The metabolite 4′‐hydroxy‐diclofenac was identified. Photolysis was used for the degradation studies and three products of diclofenac were identified (m/z of 214, 286 and 303) in aqueous solution. These results notwithstanding, no degradation products of diclofenac were found in the hospital effluent. The outcomes of this study on diclofenac reinforce the conclusions of previous investigations dealing with the determination of pharmaceuticals in the HUSM effluent, and gives evidence of the risk associated with its emission into the regional environment.