Chemometric tools improving the determination of anti-inflammatory and antiepileptic drugs in river and wastewater by solid-phase microextraction and liquid chromatography diode array detection

GIL GARCÍA, MARÍA; CAÑADA CAÑÑANA F; MARÍA CULZONI,; VERA CANDIOTI, LUCIANA; GABRIEL SIANO; MARTINEZ GALERA, MARIA; GOICOECHEA, HÉCTOR C

JOURNAL OF CHROMATOGRAPHY - A

Elsevier

Lugar: AMSTERDAM; Año: 2009 vol. 1216 p. 5489 - 5496

0021-9673

An analyticalmethod for the simultaneous determination of seven non-steroidal anti-inflammatory drugs(naproxen, ketoprofen, diclofenac, piroxicam, indomethacin, sulindac and diflunisal) and the anticonvulsantcarbamazepine in river and wastewater is reported. The method involves pre-concentration andclean-up by solid-phase microextraction using polydimethylsiloxane/divinylbenzene fibers, followed byliquid chromatography with diode array detection analysis. Owing to the fact that river water samplesdid not contain interferences and no sensitivity changes due to sample matrix were observed, externalcalibration was implemented. Standardization was also applied in order to carry out the prediction stepby preparing only two diluted standards that were subjected to the pre-concentration step and a setof standards prepared in solvent. For the analysis of wastewater samples, in contrast, it was necessaryto implement standard addition calibration in combination with the multivariate curve resolutionalternatingleast squares (MCR-ALS) algorithm, which allowed us to overcome matrix effect and exploitthe second order advantage. Recoveries ranging from 72% to 125% for all pharmaceuticals proved theaccuracy of the proposedmethod in river water samples. On the other hand, wastewater sample recoveriesranged from 83% to 140% for all pharmaceuticals, showing an acceptable performance – consideringthis sample contains no modeled interferences