| Texto completo | |
| Autor(es): |
Domingues Nazario, Carlos Eduardo
[1]
;
de Lima Gomes, Paulo Clairmont Feitosa
[1]
;
Mauro Lancas, Fernando
[1]
Número total de Autores: 3
|
| Afiliação do(s) autor(es): | [1] Univ Sao Paulo, Inst Chem Sao Carlos, Lab Chromatog, BR-13560970 Sao Carlos, SP - Brazil
Número total de Afiliações: 1
|
| Tipo de documento: | Artigo Científico |
| Fonte: | ANALYTICAL METHODS; v. 6, n. 12, p. 4181-4187, 2014. |
| Citações Web of Science: | 8 |
| Resumo | |
This paper reports on the development and validation of a simple and sensitive method that uses solid phase extraction (SPE) and liquid chromatography with ultraviolet detection to analyze fluoxetine (FLX) and norfluoxetine (NFLX) in human plasma samples. A lab-made C18 SPE phase was synthesized by using a sol-gel process employing a low-cost silica precursor. This sorbent was fully characterized by nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) to check the particles' shape, size and C18 functionalization. The lab-made C18 silica was used in the sample preparation step of human plasma by the SPE-HPLC-UV method. The method was validated in the 15 to 500 ng mL(-1) range for both FLX and NFLX using a matrix matched curve. Detection limits of 4.3 and 4.2 ng mL(-1) were obtained for FLX and NFLX, respectively. The repeatability and intermediary precision achieved varied from 7.6 to 15.0% and the accuracy ranged from -14.9 to 9.1%. The synthesized C18 sorbent was compared to commercial C18 sorbents. The average recoveries were similar (85-105%), however the lab-made C18 silica showed fewer interfering peaks in the chromatogram. After development and validation, the method using the lab-made C18 SPE was applied to plasma samples of patients under FLX treatment (n = 6). The concentrations of FLX and NFLX found in the samples varied from 46.8-215.5 and 48.0-189.9 ng mL(-1), respectively. (AU) | |
| Processo FAPESP: | 05/59360-0 - Miniaturizacao de instrumentacao analitica para tecnicas de separacao: do preparo de amostra a impressao do resultado. |
| Beneficiário: | Fernando Mauro Lanças |
| Modalidade de apoio: | Auxílio à Pesquisa - Temático |
| Processo FAPESP: | 07/03844-4 - Analise simultanea de multi-residuos de antibioticos em agua e sedimentos por extracao sorptiva em barra no modo headspace com derivatizacao in situ acoplado a gc/ms |
| Beneficiário: | Paulo Clairmont Feitosa de Lima Gomes |
| Modalidade de apoio: | Bolsas no Brasil - Doutorado Direto |