Determination of fluoxetine, norfluoxetine and their enantiomers in rat plasma and brain samples by liquid chromatography with fluorescence detection

Unceta, Nora; Barrondo, Sergio; Azúa, Iñigo Ruı́z de; Gómez‐Caballero, Alberto; Goicolea, M. Aránzazu; Sallés, Joan; Barrio, Ramón J.

doi:10.1016/j.jchromb.2007.02.008

Cited by 53 publications

(51 citation statements)

References 37 publications

(42 reference statements)

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“…The PP/LC-FD method developed here give values of accuracy and linearity close to those achieved with sample preparation methods previously described in the literature, such as liquid-liquid extraction (LLE/LC-UV), 1 solid phase extraction (SPE/LC -FD), 4 and LLE/GC-NPSD (nitrogen-phosphorus selective detector), 23 for analysis of these enantiomers in biological matrices.…”

Section: Analytical Validationsupporting

confidence: 70%

“…1222 For this purpose, several chromatographic methods (both gas chromatography, GC, and liquid chromatography, LC) have been described for the determination of FLX and NFLX enantiomers, including direct (using chiral stationary phases) and indirect (after derivatization in mobile phase) methods. [4][5][6][7][8] Moreover, as fast and reliable high throughput analysis of drug and metabolite concentrations in plasma samples is essential for pharmacokinetic, pharmacodynamic, and toxicokinetic studies, the protein precipitation method (PP) has been an ideal sample preparation technique of complex matrices, such as plasma, serum, and whole blood, for drug analysis. 9,11 In protein precipitation, acids, salts, or water miscible organic solvents are used to remove the protein by denaturation and precipitation.…”

Section: Enantioselective Analysis Of Fluoxetine and Norfluoxetine Inmentioning

confidence: 99%

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Enantioselective analysis of fluoxetine and norfluoxetine in plasma samples by protein precipitation and liquid chromatography with fluorescence detection

Bueno

Silva

Queiroz

2011

J. Braz. Chem. Soc.

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Neste trabalho, o método de precipitação de proteínas e cromatografia líquida de alta eficiência com detecção de fluorescência (PP/CLAE-fluorescência) foi desenvolvido para a análise enantioseletiva da fluoxetina e norfluoxetina em amostras de plasmas. Diferentes agentes precipitantes, como solventes orgânicos, ácidos e sais, em diferentes proporções, foram avaliados. Segundo testes calorimétricos de Bradford, dentre todos os agentes precipitantes avaliados, a acetonitrila apresentou maior eficiência, considerando o número de etapas requeridas e a porcentagem de precipitação de proteínas (99,7%), quando adicionado na proporção de 3:1 (agente precipitante: plasma, v/v). O método PP/CLAE-fluorescência apresentou limite de quantificação de 30 ng mL −1 e intervalo linear de 30 a 1000 ng mL −1 com coeficientes de regressão linear acima de 0,9973 para os quatro enantiômeros. Em conclusão, o método PP/CLAE-fluorescência padronizado e validado proposto neste estudo foi aplicado com sucesso na análise de amostras de plasma de pacientes em terapia com a fluoxetina.In this study, the enantioselective analysis of fluoxetine and norfluoxetine in plasma samples was performed by the protein precipitation method and high performance liquid chromatography with fluorescence detection (PP/LC-FD). Different precipitating agents -organic solvents, acids, and salts -in several proportions were available. The Bradford colorimetric method employed for evaluation of the efficiency of protein precipitation, has shown that for the sake of simplicity and percentage of protein precipitation (99.7%), acetonitrile was most effective when added at a ratio of 3:1 (acetonitrile/plasma, v/v). The quantification limit of the PP/LC-FD method was 30 ng mL −1 for the four enantiomers. The response of the proposed method was linear over a dynamic range from LOQ to 1000 ng mL −1 , with correlation coefficients higher than 0.9973. In conclusion, the PP/LC-FD method can be successfully used to analyze plasma samples from ageing patients undergoing therapy with fluoxetine.

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Section: Analytical Validationsupporting

confidence: 70%

Section: Enantioselective Analysis Of Fluoxetine and Norfluoxetine Inmentioning

confidence: 99%

Enantioselective analysis of fluoxetine and norfluoxetine in plasma samples by protein precipitation and liquid chromatography with fluorescence detection

Bueno

Silva

Queiroz

2011

J. Braz. Chem. Soc.

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“…The analysis of mass spectra and literature data [36] allows to assign the structure of 3-phenyl-3-hydroxypropylamine (m/z 152) to the degradation product of R F ∼0.24 (P-A), and the structure of 4-trifluoromethylphenol (m/z 164) to degradation product of R F ∼0.55 (P-B). The signal on a mass spectra of m/z = 310 was identified as fluoxetine, and an additional signal of m/z = 351 as an adduct of fluoxetine and acetonitrile present in mobile phase of chromatographic separation [3] (Figs 6-8). The scheme of fluoxetine photodegradation in the presence of metal ions may be proposed as a result of the study conducted (Fig.…”

Section: Identification Of Degradation Productsmentioning

confidence: 99%

“…Fluoxetine was determined in the presence of its metabolites and other drugs in biological samples [3][4][5][6] and in pharmaceutical preparations [7][8][9] by high-performance liquid chromatography (HPLC) with UV detection. Liquid chromatography with MS detection [10][11][12][13][14], gas chromatography (GC)-MS [15][16][17][18], and capillary electrophoresis [19] were mainly used for the determination of fluoxetine in biological samples.…”

Section: Introductionmentioning

confidence: 99%

Determination of fluoxetine in the presence of photodegradation products appearing during UVA irradiation in a solid phase by chromatographic-densitometric method, kinetics and identification of photoproducts

Maślanka¹,

Hubicka²,

Krzek³

et al. 2013

Acta Chromatographica

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Summary. An effect of ultraviolet A (UVA) radiation on fluoxetine stability in solid phase with and without the presence of selected metal ions was studied using the chromatographic-densitometric method. Silica gel TLC F 254 plates were used as the stationary phase and chloroform-methanol-ammonia 25% ( The liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS) method was applied for the identification of decomposition products noting the presence of 3-phenyl-3-hydroxypropylamine and 4-trifluoromethylphenol.

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“…Direct and indirect chiral separation methods have been reported for fluoxetine and/or norfluoxetine based on GC [15,16] and HPLC using chiral stationary phases (CSPs) [17][18][19][20][21][22] or chiral derivatization reagents (CDRs) [23,24] (Supporting Information Table S1). Previous methods for indirect enantiomeric separation of fluoxetine were based on chiral derivatization using R-naphthyl ethyl isocyanate, followed by chromatographic separation on normal-phase chromatography coupled to fluorescence detection [23,24].…”

Section: Introductionmentioning

confidence: 99%

Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1R‐(–)‐menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time‐of‐flight mass spectrometry

Zhao

Jin

Shin

et al. 2016

J of Separation Science

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Here we describe a simple and sensitive analytical method for the enantioselective quantification of fluoxetine in mouse serum using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry. The sample preparation method included a simple deproteinization with acetonitrile in 50 μL of serum, followed by derivatization of the extracts in 50 μL of 2 mM 1R-(-)-menthyl chloroformate at 45ºC for 55 min. These conditions were statistically optimized through response surface methodology using a central composite design. Under the optimized conditions, neither racemization nor kinetic resolution occurred. The derivatized diastereomers were readily resolved on a conventional sub-2 μm C18 column under a simple gradient elution of aqueous methanol containing 0.1% formic acid. The established method was validated and found to be linear, precise, and accurate over the concentration range of 5.0-1000.0 ng/mL for both R and S enantiomers (r(2) > 0.993). Stability tests of the prepared samples at three different concentration levels showed that the R- and S-fluoxetine derivatives were relatively stable for 48 h. No significant matrix effects were observed. Last, the developed method was successfully used for enantiomeric analysis of real serum samples collected at a number of time points from mice administered with racemic fluoxetine.

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Determination of fluoxetine, norfluoxetine and their enantiomers in rat plasma and brain samples by liquid chromatography with fluorescence detection

Cited by 53 publications

References 37 publications

Enantioselective analysis of fluoxetine and norfluoxetine in plasma samples by protein precipitation and liquid chromatography with fluorescence detection

Enantioselective analysis of fluoxetine and norfluoxetine in plasma samples by protein precipitation and liquid chromatography with fluorescence detection

Determination of fluoxetine in the presence of photodegradation products appearing during UVA irradiation in a solid phase by chromatographic-densitometric method, kinetics and identification of photoproducts

Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1R‐(–)‐menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time‐of‐flight mass spectrometry

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