Development of a solid phase extraction for 13 ‘new’ generation antidepressants and their active metabolites for gas chromatographic–mass spectrometric analysis

Wille, Sarah M. R.; Maudens, Kristof E.; Peteghem, Carlos H. Van; Lambert, Willy E.

doi:10.1016/j.chroma.2005.08.059

Cited by 139 publications

(67 citation statements)

References 39 publications

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“…Methods capable of separating enantiomers of venlafaxine and O-desmethylvenlafaxine have been reported based on capillary electrophoresis [5][6][7][8][9][10][11][12][13] and HPLC-ESI/MS [14]. Thus, the aim of the present work was to establish a simple, accurate, rapid and sensitive LC-MS/MS method with a lower limit of quantification (LLOQ) of 0.5 ng/mL using a very low volume (50μL) of rabbit plasma.…”

Section: Introductionmentioning

confidence: 99%

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

Reddy¹

2011

J Anal Bioanal Tech

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A highly senstive and rapid LC-MS/MS method has been developed and validated for the estimation of desvenlafaxine in rabbit plasma. The chromatographic separation was performed with 0.2% formic acid: methanol at flow rate of 0.4 mL/min on Symmetry Shield RP18 column with a total run time of 3.0 min. TheMS/MS ion transitions monitored were 263.90 58.10 for desvenlafaxine and 281.30 86.10 for IS (metaprolol). Method validation and pre-clinical sample analysis were performed as per FDA guide lines and the results met the acceptance crieteria. The lower limit of quantification achieved was 0.5 ng/mL and the linearity was observed from 0.5 to 1500ng/mL. This novel method has been applied to pharmacokinetic study of desvenlafaxine in rabbits. Page 2 of 6 10ASvp) and auto-sampler (SIL-HTC) along with a system controller (SCL-10Avp) was used to inject 2 μL aliquots of the processed samples on a Symmetry Shield RP18 column (50 x 4.6 mm, 3.5 μm, Waters Corporation, Ireland, UK), which was kept at ambient temperature (24 ± 2°C). The isocratic mobile phase, a mixture of 0.2% formic acid and methanol mixture (20:80, v/v) was filtered through a 0.45 μm membrane filter (Millipore) and then degassed ultrasonically for 5 min was delivered at a flow rate of 0.40 mL/min into the mass spectrometer electro spray ionization chamber. Mass spectrometry operating conditionsQuantification was achieved by MS/MS detection in positive ion mode for analyte and IS using a MDS Sciex (Foster City, CA, USA) API 4000 mass spectrometer, equipped with a Turboionspray™ interface at 500°C. The common parameters, i.e. curtain gas, nebulizer gas, auxillary gas and collision gas, were set at 10, 35, 40 and 6 psi, respectively. The compounds parameters, i.e. declustering potential (DP), collision energy (CE), collision exit potential (CXP) and entrance potential (EP) for DVS and IS were 60, 43, 8, 10 V and 44, 26, 8, 10 V, respectively. Detection of the ions was performed in the multiple reaction monitoring (MRM) mode, monitoring the transition of the m/z 263.90 precursor ion to the m/z 58.10 product ion for DVS and m/z 281.30 precursor ion to the m/z 86.10 product ion for IS. Quadrupole Q1 was set on low resolution where as Q3 was set on unit resolution. The analytical data were processed by Analyst software (version 1.4.2). Preparation of stock and standard solutionsPrimary stock solutions of DVS for preparation of standard and quality control (QC) samples were prepared from separate weighing. The primary stock solutions were prepared in methanol (1000 μg/mL). The IS stock solution of 1000 μg/mL was prepared in methanol. The stock solutions of DVS and IS were stored at 4°C, which were found to be stable for one month (data not shown) and successively diluted with methanol to prepare working solutions to prepare the calibration curve (CC). Another set of working stock solutions of DVS were made in methanol (from primary stock) for preparation of QC samples. Working stock solutions were stored at approximately 4°C for a week (data not shown). A...

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Section: Introductionmentioning

confidence: 99%

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

Reddy¹

2011

J Anal Bioanal Tech

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“…Several methods have been developed for the determination of paroxetine in plasma, including HPLC with ultraviolet [5,6], fluorescence (without or with derivatization using dansylchloride) [7][8][9], mass spectroscopy (MS) [10,11], diode array detection [12,13], or gas chromatography with MS detection [14,15] and applied therapeutic drug level monitoring. Only few methods have been published for the simultaneous determination of paroxetine and its metabolites in plasma, using HPLC with UV [2,16]; or applied to pharmacokinetic, therapeutic drug level monitoring, toxicological screening or forensic cases [17].…”

Section: Introductionmentioning

confidence: 99%

Determination of Paroxetine in Pharmaceutical Preparations Using HPLC with Electrochemical Detection

Agrawal¹

2013

TOACJ

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A reliable and sensitive high performance liquid chromatographic method for the determination of widely prescribed antidepressant has been developed. Paroxetine is a potent selective serotonin reuptake inhibitor used for the treatment of depression and various mood disorders. The optimum mobile phase was prepared using a combination of 40% acetonitrile and phosphate buffer 0.01 M to pH 3 and running under isocratic mode at a flow rate of 1.0 ml/min. with electrochemical detection at 0.9V. The applicability of the developed method is in the field of quality control as well as for monitoring the level of drug at various concentrations during synthesis of the parent drug. The suggested methodology was validated following the guidelines of the FDA in terms of: sensitivity (LOD and LOQ, 0.005 and 0.01 ng/mL, respectively), linearity between 0.5 -50 ng/mL (r 2 > 0.9999), inter-and intraday precision (< 0.259% and < 0.538%), robustness (less than 5.0%) and recovery (99.7 -100.7%). The developed method is specific, rapid (less than 10 min), precise, reliable, accurate, cheap and suitable for routine analysis for the determination of paroxetine in pharmaceutical preparations.

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“…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. In general, urine is used as primary specimen in forensic screening analyses, owing to the higher concentrations and longer detection window of compounds of interest compared to whole blood.…”

Section: Introductionmentioning

confidence: 99%

“…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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Development of a solid phase extraction for 13 ‘new’ generation antidepressants and their active metabolites for gas chromatographic–mass spectrometric analysis

Cited by 139 publications

References 39 publications

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

Determination of Paroxetine in Pharmaceutical Preparations Using HPLC with Electrochemical Detection

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

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