Validated semiquantitative/quantitative screening of 51 drugs in whole blood as silylated derivatives by gas chromatography-selected ion monitoring mass spectrometry and gas chromatography electron capture detection

Gunnar, Teemu; Mykkänen, Sirpa; Ariniemi, Kari; Lillsunde, Pirjo

doi:10.1016/j.jchromb.2004.04.005

Cited by 111 publications

(82 citation statements)

References 22 publications

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“…LLE was also efficiently applied to cocaine and its metabolites determination in other matrices including hair (Kintz & Mangin, 1995), nails (Engelhart & Jenkins, 2002), serum (Williams et al, 1996), plasma (Dawling et al, 1990), whole blood (Gunnar et al, 2004) and organ tissues (Hime et al, 1991).…”

Section: Analytementioning

confidence: 99%

Chromatographic Methodologies for Analysis of Cocaine and Its Metabolites in Biological Matrices

Valente¹,

Carvalho²,

Bastos³

et al. 2012

Gas Chromatography - Biochemicals, Narcotics and Essential Oils

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Section: Analytementioning

confidence: 99%

Chromatographic Methodologies for Analysis of Cocaine and Its Metabolites in Biological Matrices

Valente¹,

Carvalho²,

Bastos³

et al. 2012

Gas Chromatography - Biochemicals, Narcotics and Essential Oils

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“…Such an approach is the best choice in the analysis of many compounds that differ in structure and properties [12]. Gas chromatography hyphenated with mass spectrometry (GC-MS) is, however, also used, even in the analysis of relatively complex mixtures of pharmaceuticals in both the environmental [13] and biological samples [14]. The detailed study concerning the synthesis of derivatives of some pharmaceuticals for GC-MS analyses was published recently [15].…”

Section: Introductionmentioning

confidence: 99%

The derivatization and analysis of anticancer pharmaceuticals in the presence of tricyclic antidepressants by gas chromatography

Haliński

Smigiel

Czerwicka

et al. 2014

Acta Chromatographica

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Summary. The evaluation of several derivatization procedures for the gas chromatographic analysis of selected anticancer pharmaceuticals (cyclophosphamide, iphosphamide, flutamide, chlorambucil, and melphalan) in the presence of tricyclic antidepressants was carried out. Among the methods, concerning trimethylsilylation, tertbutyldimethylsilylation, and methylation, the most useful was methylation using (trimethylsilyl)diazomethane (TMSD), which is a safe alternative for the common reaction with diazomethane. Most of the anticancer drugs were unstable during derivatization using silylating agents, while antidepressants were stable in all tested conditions. Melphalan was the only compound, for which the results of all tested procedures were not satisfying. The TMSD-based procedure was validated, giving the results possibly suitable for the screening purposes in contaminated environmental samples.

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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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Validated semiquantitative/quantitative screening of 51 drugs in whole blood as silylated derivatives by gas chromatography-selected ion monitoring mass spectrometry and gas chromatography electron capture detection

Cited by 111 publications

References 22 publications

Chromatographic Methodologies for Analysis of Cocaine and Its Metabolites in Biological Matrices

Chromatographic Methodologies for Analysis of Cocaine and Its Metabolites in Biological Matrices

The derivatization and analysis of anticancer pharmaceuticals in the presence of tricyclic antidepressants by gas chromatography

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

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