| Full text | |
| Author(s): |
Domingues Nazario, Carlos Eduardo
[1]
;
de Lima Gomes, Paulo Clairmont Feitosa
[1]
;
Mauro Lancas, Fernando
[1]
Total Authors: 3
|
| Affiliation: | [1] Univ Sao Paulo, Inst Chem Sao Carlos, Lab Chromatog, BR-13560970 Sao Carlos, SP - Brazil
Total Affiliations: 1
|
| Document type: | Journal article |
| Source: | ANALYTICAL METHODS; v. 6, n. 12, p. 4181-4187, 2014. |
| Web of Science Citations: | 8 |
| Abstract | |
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) | |
| FAPESP's process: | 05/59360-0 - Miniaturization of analytical instrumentation for separation techniques: sample preparation and printing of result |
| Grantee: | Fernando Mauro Lanças |
| Support Opportunities: | Research Projects - Thematic Grants |
| FAPESP's process: | 07/03844-4 - Simultaneous analysis of multi-residue antibiotics in water and sediments by headspace bar sorptive extraction with in situ derivatization coupled to GC / MS |
| Grantee: | Paulo Clairmont Feitosa de Lima Gomes |
| Support Opportunities: | Scholarships in Brazil - Doctorate (Direct) |