Determination of fluoxetine and norfluoxetine in human plasma by high-performance liquid chromatography with ultraviolet detection in psychiatric patients

LLerena, Adrián; Dorado, Pedro; Berecz, Roland; González, Antonio; Norberto, Marı́a Jesús; Rubia, Alfredo de la; Cáceres, Macarena C.

doi:10.1016/s1570-0232(02)00486-5

Cited by 55 publications

(31 citation statements)

References 27 publications

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“…(S)-FLX ex-hibited a longer duration of action and is approximately 1.5 times more potent than R-enantiomer and displays a threefold longer duration of action (Grodner and Sitkiewicz, 2013). Chromatographic methods, as LC or GC with chiral columns or chiral additives into mobile phase are typical for the determination of the FLX enantiomers (Lerena et al, 2003;Li et al, 2004;Mifsud and Sqhendo, 2012;Yu et al, 2012;Ribeiro et al, 2013). Few studies of FLX chiral analysis using non-chromatography methods such as capillary electrophoresis were published (Asensi-Bernardi et al, 2013) and NMR (Ali et al, 2005;Shamsipur et al, 2007).…”

Section: Introductionmentioning

confidence: 99%

Determination of enantiomeric composition of fluoxetine by synchronous fluorescence spectrometry coupled with multivariate calibration in biological samples

Poláček

Májek

Sádecká

2016

Acta Chimica Slovaca

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This paper presents rapid and low cost analytical method for the determination of the fluoxetine enantiomeric composition in biological samples (urine). The combination of synchronous fluorescence spectrometry and inverse multivariate calibration methods was used. The chiral recognition of the fluoxetine was based on the creating of the diastereomeric complexes with -cyclodextrin. A net analytical signal of diastereomeric complexes was obtained by the addition of aliquot part of urine into calibration and validation sets. This step ensures the elimination of the urine matrix effect. The synchronous fluorescence spectra at the constant wavelength differences (∆λ) of 30 and 50 nm, based on RMS %RE values, were chosen for chemometric analysis. Principal component regression (PCR) and partial least square method (PLS) were compared to determine the enantiomeric composition. The most suitable results were provided by the PLS model constructed from the synchronous data at ∆λ = 50 nm. The calculated figure of merit was used for validation of proposed method.

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Section: Introductionmentioning

confidence: 99%

Determination of enantiomeric composition of fluoxetine by synchronous fluorescence spectrometry coupled with multivariate calibration in biological samples

Poláček

Májek

Sádecká

2016

Acta Chimica Slovaca

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“…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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“…Several methods have been published for the analysis of fluoxetine and norfluoxetine in pharmaceutical formulations, in theurapeutic drug monitoring, in biological fluids, and in postmortem tissues, including gas chromatography (5-8), gas chromatographic-mass spectrometric detection (GC-MS) (4,(8)(9)(10)(11)(12)(13), high performance liquid chromatographic (HPLC) separation (14)(15)(16)(17)(18)(19)(20)(21)(22), liquid chromatography separation with mass spectrometric detection (LC-MS) (23)(24)(25) and capillary electrophoresis (26). Liquid-liquid extraction (4,7,10,16,17), solid phase extraction (SPE) (5,11,13,18), and solid phase microextraction (SPME) (12) are the most common sample preparation techniques to analyze fluoxetine and norfluoxetine in biological fluids.…”

Section: Introductionmentioning

confidence: 99%

GC-MS analysis of fluoxetine and its active metabolite norfluoxetine in human urine

Açıkkol¹

2010

mpj

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A gas chromatographic-mass spectrometric (GC-MS) method was developed for detection of fluoxetine and its active metabolite norfluoxetine in urine. Liquid and solid phase extraction were applied to urine samples using maprotiline as an internal standard (IS). The GC-MS analysis were carried out using HP-5MS capillary column. The linearity ranges of the method were 5-75 ng mL -1 for fluoxetine and 6-125 ng mL -1 for norfluoxetine by solid phase extraction (SPE), and 10-80 ng mL -1 for fluoxetine and also norfluoxetine by liquid-liquid extraction (LLE). Also the range of detection limits were between 1-10 ng mL -1 , the range of quantification limits were between 5-10 ng mL -1 for fluoxetine and norfluoxetine by both SPE and LLE. The range of recoveries were between 87 -109 % by both SPE and LLE for analytes. The developed method allowed clinical and toxicological analysis of fluoxetine and norfluoxetine in urine samples.KEY WORDS: Fluoxetine; Norfluoxetine; Gas Chromatography-Mass Spectrometry; LiquidLiquid Extraction; Solid-Phase Extraction.Münevver Aç kkol 1 , Dilek Salk m 1 GC-MS analysis of fluoxetine and its active metabolite norfluoxetine in human urine DOI: 10.12991/201014456 99 Açıkkol ve Salkım et al. Marmara Pharm J 14: 98-103, 2010. plicity, sensitivity, reproducide nature and low cost. There were only a few published methods about the simultaneous GC-MS analysis of fluoxetine and norfluoxetine in urine.Therefore, the presented study was designed for a GC-MS method for the simultaneous determination of fluoxetine and norfluoxetine in urine using maprotiline as an internal standard (IS) with a simple LLE and SPE procedure. MATERIALS AND METHODS Chemicals and reagentsFluoxetine hydrochloride was purchased from Sigma Aldrich (Steinheim, Germany) and kindly supplied by Abdi Ibrahim Pharma A.G (Istanbul, Turkey). Norfluoxetine hydrochloride was purchased from Sigma Aldrich (Steinheim, Germany). Maprotiline hydrochloride (IS) was kindly supplied by Novartis Pharma A.G (Istanbul, Turkey).Ammonia solution (25%), hexane, dichloromethane, ethyl acetate, acetic anhydride, pyridine, methanol and isopropanol were purchased from Merck (Darmstadt, Germany). Purity of all solvents are HPLC grade. Urine samplesUrine samples were collected from healthy volunteers whereas clinical samples from patients (14 females and 6 males; Aged 18-64) submitted fluoxetine treatment at Istanbul University Medicine Faculty of Cerrahpasa Department of Psychiatry. Samples were collected approximately 12 hours after the administration of the daily dose of 20 mg of fluoxetine from patients treated constantly for at least 2 weeks. The urine samples stored in appropriate polytetrafluoro ethylene (PTPE) flasks at -20ºC until analyzed and were found to be stable for at least 1 month. The patients gave their informed consent for these analyses. The study protocol was approved by the Ethics Committee of The Faculty of Cerrahpasa Medicine in Istanbul University. Preparation stock and calibration standardsStock solutions of fluoxet...

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Determination of fluoxetine and norfluoxetine in human plasma by high-performance liquid chromatography with ultraviolet detection in psychiatric patients

Cited by 55 publications

References 27 publications

Determination of enantiomeric composition of fluoxetine by synchronous fluorescence spectrometry coupled with multivariate calibration in biological samples

Determination of enantiomeric composition of fluoxetine by synchronous fluorescence spectrometry coupled with multivariate calibration in biological samples

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

GC-MS analysis of fluoxetine and its active metabolite norfluoxetine in human urine

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