Development and validation of analytical methodology for determination of pharmaceutical compounds in surface and surface treated water samples by ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) / Desenvolvimento e validação de metodologia analítica para a determinação de fármacos em amostras de água, superficial e tratada, utilizando a cromatografia líquida de ultra performance acoplada à espectrometria de massas Tandem (UPLC-MS/MS)

Valéria Chiérice Rodrigues

The relevant concept of sustainability of the present day leads people to think about the treatment of natural resources and particularly in the quanlity and scarcity of water. The serious problems regarding the management of municipal waste in the country, from production, collection and disposal are the challenges facing municipalities and society in general. The increasing use of pharmaceutical drugs most abundant generates a demand for waste that eventually reach the river beds. With advancement of technologies and know you can monitor the waste that directly and indirectly affect the waters of river basins. The objective of this study was to develop and validade analytical methods for residues of drugs (aspirin, sodium diclofenac, paracetamol, ibuprofen and fenoprofen) in water using ultra performance liquida chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). We used two different mobile phases. For the drugs paracetamol and diclofenac was used as mobile phase water:methanol (1:1, v/v) with addition of formic acid in positive electrospray ionization mode. For drugs acetyl salicylic acid, ibuprofen and fenoprofen was used mobile phase water:methanol (1:1, v/v) with addition of ammonium acetate and negative electrospray ionization mode. The performance of the method was evaluated on the following parameters: specificity and selectivity, working range, lineariry, limit of detection and limit of quantification, accuracy, ruggedness and uncertainty measurement. The result obtained proved the suitability of the method for fit purpose. The values obtained for the decision limit (ccα) and detection capability (ccβ) were 0.21 and 0.34 μg L-1, diclofenac 2.42 and 3.24 μgL-1, ASA 1.56 and 2.45 μgL-1, respectively. The methodology was applied in the characterization of samples of surface water (raw) and treated from catchment areas and water treatment basin of Paraíba do sul were two distinct collections, September/2011 and November 2010 in the municipalities of Guararema, São José dos Campos, Taubaté and Pindamonhangaba. In 32,2% of all samples, five samples of 16 raw water samples, residues were found for paracetamol. The results were presented in a concentration range from 0.10 to 0.50 μg L-1.

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