Sample as solid support in MSPD: A new possibility for determination of pharmaceuticals, personal care and
Maristela B R Cerqueira1, Karina L Soares1, Sergiane S Caldas1
1Post-graduation Program in Technological and Environmental Chemistry, Escola de Química e Alimentos, Laboratório de Análise de Compostos Orgânicos e Metais (LACOM), Universidade Federal do Rio Grande-FURG, Av Itália, Km 8, s/n, Rio Grande, Rio Grande, do Sul State, 96201-900, Brazil.
Abstract:
A method based on matrix-solid phase dispersion (MSPD), focused on the principles of green analytical chemistry, aimed at the use of alternative solid supports and less toxic solvents, was developed for the simultaneous determination of 19 pharmaceuticals, 4 personal care products (PPCPs) and 4 degradation products in sewage sludge samples. Higher recoveries were achieved when 2 g sample was macerated for 5 min in a glass mortar, transferred to a centrifuge tube, and 1 min vortex agitation with 5 mL methanol. The performance of the method was evaluated through linearity, recovery, precision (intra-day), method detection and quantification limits (MDL and MQL) and matrix effect. The calibration curves prepared in methanol and in the matrix extract showed a correlation coefficient ranging from 0.98 to 0.99. MQL values ranged from 1.25 to 1250 ng g-1. Recoveries between 50 and 120% were reached with RSDs lower than 20% for most compounds. The method presented low and medium matrix effects for most analytes. This method was successfully applied to real samples and of the 27 compounds determined, amitriptyline, carbamazepine, diclofenac, haloperidol, ketoconazole, miconazole, albendazole, mebendazole, thiabendazole, triclosan and triclocarban were detected in concentrations between 2.5 and 5400 ng g-1.
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