Analysis of fluoxetine and norfluoxetine in human plasma by HPLC-UV using a high purity C18 silica-based SPE sorbent

Autor(es)

Domingues Nazario, Carlos Eduardo ^[1] ; de Lima Gomes, Paulo Clairmont Feitosa ^[1] ; Mauro Lancas, Fernando ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Inst Chem Sao Carlos, Lab Chromatog, BR-13560970 Sao Carlos, SP - Brazil

• 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 - Miniaturização de instrumentação analítica para técnicas de separação: do preparo de amostra a impressão do resultado
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 07/03844-4 - Análise simultânea de multi-resíduos de antibióticos em água e sedimentos por extração sorptiva em barra no modo headspace com derivatização "in situ" acoplado a GC/MS
• Beneficiário: Paulo Clairmont Feitosa de Lima Gomes
• Modalidade de apoio: Bolsas no Brasil - Doutorado Direto