Optimization and validation of a method using SPE and LC-APCI-MS/MS for determination of pharmaceuticals in surface and public supply water

Autor:	Ednei Gilberto Primel, Maicon R. F. Sampaio, Débora Tomasini, Sergiane Souza Caldas, Fábio Ferreira Gonçalves, Natiele Kleemann, Liziane V. Cardoso
Jazyk:	angličtina
Rok vydání:	2011
Předmět:	Detection limit Public supply Chromatography Liquid chromatography–mass spectrometry Chemistry Lc apci ms ms LC-APCI-MS/MS Analytical chemistry method validation General Chemistry Solid phase extraction SPE emergent contaminants
Zdroj:	Journal of the Brazilian Chemical Society v.22 n.10 2011 Journal of the Brazilian Chemical Society Sociedade Brasileira de Química (SBQ) instacron:SBQ Repositório Institucional da FURG (RI FURG) Universidade Federal do Rio Grande (FURG) instacron:FURG Journal of the Brazilian Chemical Society, Volume: 22, Issue: 10, Pages: 1944-1952, Published: OCT 2011
Popis:	In this work, an analytical method based on solid phase extraction (SPE) and liquid chromatography tandem mass spectrometry (LC-APCI-MS/MS) was developed and validated for the determination and confirmation of five pharmaceuticals in water samples. The limits of detection (LOD) ranged from 0.053 to 0.53 µg L-1 and the limits of quantification (LOQ) from 0.16 to 1.6 µg L-1. Good linearity was obtained with r > 0.99 for all compounds. The recoveries of the compounds ranged from 70 to 120% with relative standard deviations (RSD) below 20% for all. Through multiple reactions monitoring (MRM) two different transitions, precursor ion-product ion, were selected for each pharmaceutical. Neste trabalho, foi desenvolvido e validado um método analítico baseado na extração em fase sólida (SPE) e cromatografia líquida acoplada a espectrometria de massas em tandem (LC-APCI-MS/MS) para a determinação e confirmação de cinco fármacos em amostras de água. Os limites de detecção (LOD) variaram de 0,053 a 0,53 µg L-1 e os limites de quantificação (LOQ) de 0,16 a 1,6 µg L-1. Foi obtida boa linearidade com r > 0,99 para todos os compostos. As recuperações dos compostos variaram de 70 a 120%, com desvios padrão relativos (RSD) menores que 20% para todos. Através do monitoramento de reações múltiplas (MRM), foram selecionadas duas transições diferentes íon precursor-íon produto para cada fármaco.
Databáze:	OpenAIRE
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