Porous graphitic carbon chromatography–tandem mass spectrometry for the study of isoprostanes in human cerebrospinal fluid

Bohnstedt, Kristina Claeson; Karlberg, Bo; Basun, Hans; Schmidt, Staffan

doi:10.1016/j.jchromb.2005.02.023

Cited by 12 publications

(6 citation statements)

References 20 publications

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“…The ability of this graphitic material to retain small polar molecules is superior to that of silica-based sorbents (Gamelin et al, 1998;Fleming et al, 1993;Remaud et al, 2005;Ayrton et al, 1995;Gu and Lim, 1990;Cantu et al, 2001;Mazan et al, 2002;Gaudin et al, 2002;Jackson and Carr, 2002;Hanai, 2003;Antonio et al, 2007;Pereira et al, 2007;Merelli et al, 2007;Tachon et al, 2007;Xia et al, 2006;Roy et al, 2006;Bohnstedt et al, 2005;Reepmeyer et al, 2005;Xing et al, 2004;Thiebaut et al, 2006;Vial et al, 2001;Lepont et al, 2001;Holmgren et al, 2005). Moreover, porous graphitic carbon proved to be chemically and pH stable, and an inert stationary phase.…”

Section: Development Of a Pgc-hplc-ms/ms Methodsmentioning

confidence: 99%

A new, validated HPLC‐MS/MS method for the simultaneous determination of the anti‐cancer agent capecitabine and its metabolites: 5′‐deoxy‐5‐fluorocytidine, 5′‐deoxy‐5‐fluorouridine, 5‐fluorouracil and 5‐fluorodihydrouracil, in human plasma

Vainchtein

Rosing

Schellens

et al. 2009

Biomedical Chromatography

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A rapid and selective liquid chromatography/tandem mass spectrometric method was developed for the simultaneous determination of capecitabine and its metabolites 5'-deoxy-5-fluorocytidine (5'-DFCR), 5'-deoxy-5-fluorouracil (5'-DFUR), 5-fluorouracil (5-FU) and dihydro-5-fluorouracil (FUH(2)) in human plasma. A 200 microL human plasma aliquot was spiked with a mixture of internal standards fludarabine and 5-chlorouracil. A single-step protein precipitation method was employed using 10% (v/v) trichloroacetic acid in water to separate analytes from bio-matrices. Volumes of 20 microL of the supernatant were directly injected onto the HPLC system. Separation was achieved on a 30 x 2.1 mm Hypercarb (porous graphitic carbon) column using a gradient by mixing 10 mm ammonium acetate and acetonitrile-2-propanol-tetrahydrofuran (1 : 3 : 2.25, v/v/v). The detection was performed using a Finnigan TSQ Quantum Ultra equipped with the electrospray ion source operated in positive and negative mode. The assay quantifies a range from 10 to 1000 ng/mL for capecitabine, from 10 to 5000 ng/mL for 5'-DFCR and 5'-DFUR, and from 50 to 5000 ng/mL for 5-FU and FUH(2) using a plasma sample of 200 microL. Correlation coefficients (r(2)) of the calibration curves in human plasma were better than 0.99 for all compounds. At all concentration levels, deviations of measured concentrations from nominal concentration were between -4.41 and 3.65% with CV values less than 12.0% for capecitabine, between -7.00 and 6.59% with CV values less than 13.0 for 5'-DFUR, between -3.25 and 4.11% with CV values less than 9.34% for 5'-DFCR, between -5.54 and 5.91% with CV values less than 9.69% for 5-FU and between -4.26 and 6.86% with CV values less than 14.9% for FUH(2). The described method was successfully applied for the evaluation of the pharmacokinetic profile of capecitabine and its metabolites in plasma of treated cancer patients.

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Section: Development Of a Pgc-hplc-ms/ms Methodsmentioning

confidence: 99%

A new, validated HPLC‐MS/MS method for the simultaneous determination of the anti‐cancer agent capecitabine and its metabolites: 5′‐deoxy‐5‐fluorocytidine, 5′‐deoxy‐5‐fluorouridine, 5‐fluorouracil and 5‐fluorodihydrouracil, in human plasma

Vainchtein

Rosing

Schellens

et al. 2009

Biomedical Chromatography

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“…The composition of the mobile phase is an important factor that affects the ESI processes [31]. In order to reduce signal suppression, well-ionized analytes as well as a high content of organic modifier in the mobile phase are favorable.…”

Section: Second Dimension (Rp)mentioning

confidence: 99%

Fast and simple online sample preparation coupled with capillary LC‐MS/MS for determination of prostaglandins in cell culture supernatants

Rinne¹,

Kleiveland

Kassem

et al. 2007

J of Separation Science

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An online 2-D strong cation exchange (SCX)-RP capillary liquid chromatographic (cLC) method with IT mass spectrometric (IT-MS/MS) detection for the simultaneous determination of prostaglandin (PG) A(1), PGD(2), PGE(1), PGE(2), PGF(2a), 6-keto-(6k)PGF(1a), and 15-Delta(12,14)-deoxy-PGJ(2) (15dPGJ(2)) in cell culture supernatants was developed and validated. Pretreatment of the cell culture supernatants included dilution and filtration, and the analysis time including all sample preparation steps was less than 50 min per sample. Peptides/proteins contained in the matrix were removed by the SCX column. LODs in the range of 0.4-2.2 ng/mL cell culture supernatant, recoveries higher than 80% and within- and between-day precisions of less than 30% RSDs were obtained. Human mesenchymal stem cells (hMSCs) were stimulated with cytokine-containing supernatants derived from activated T lymphocytes, and PG production was analyzed using the developed method. PGE(2 )was found in cultures from both untreated and stimulated hMSCs, while PGE(1) was present above the detection limit only in stimulated cells.

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“…Although PGC columns have been used in the separation of diastereomers 5,13,14 and polar analytes, 7,19-21 only a few applications have been reported for bioanalytical quantitation. [8][9][10][11][12][13][14] It is essential to establish the ruggedness of the PGC column, in terms of maintenance of its separation capability, sensitivity, peak symmetry and back pressure, when used for extended period for analyzing biological samples by LC/MS/MS. In our investigation, we applied minimal clean-up of the plasma samples using only the simple acetonitrile-precipitation procedure in order to test the column ruggedness by injecting crude extracts.…”

Section: Resultsmentioning

confidence: 99%

“…This stationary phase has been used for the separation of positional isomers, such as equine conjugated estrogens, equilin sulfate and Δ8,9‐dehydroestrone sulfate,6 as well as for separating some polar compounds, such as nucleosides and their mono‐, di‐, and triphosphates 7. To our knowledge, there are only a few published methods using a PGC column for bioanalytical quantitation, such as the separation and quantitation of 5‐fluorouracil, 5‐fluorodihydrouracil and its prodrug ftorafur in serum,8, 9 guanidine compounds in serum,10, 11 glutathione in plasma,12 and isoprostanes in urine and cerebrospinal fluid 13, 14…”

mentioning

confidence: 99%

Utility of porous graphitic carbon stationary phase in quantitative liquid chromatography/tandem mass spectrometry bioanalysis: quantitation of diastereomers in plasma

Xia

Jemal

Zheng

et al. 2006

Rapid Comm Mass Spectrometry

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A major challenge in selecting an appropriate stationary phase for diastereomeric separation is that it is difficult to predict which of the commercially available stationary phases could achieve the required liquid chromatographic (LC) separation. This work describes the selection and evaluation of a porous graphitic carbon (PGC) column coupled with tandem mass spectrometry (MS/MS) for the simultaneous quantitation of an experimental drug candidate (I), its two diastereomeric metabolites (II and III), and its demethylated metabolite (IV) in rat plasma. In addition, we investigated the PGC column for the separation of another drug candidate (VI), its two diastereomeric metabolites (VII and VIII) and its ketone metabolite (IX). The PGC column showed excellent chromatographic resolution for the two diastereomers II and III, as well as for VII and VIII. In contrast, the required resolution for the diastereomers II and III could not be achieved using silica-bonded C(18), C(30), phenyl, perfluorinated, polar embedded and polar end-capped phases. The PGC column showed ruggedness with excellent reproducibility of retention times, peak symmetry and response over a period of more than 400 injections of a plasma acetonitrile-precipitation extract. Excellent accuracy and precision were achieved, with accuracy of 94-108% and intra- and inter-run precision within 9%. This work indicates that PGC is a valuable addition to the repertoire of LC columns used for quantitative LC/MS/MS bioanalysis, especially where the separation and quantitation of diastereomeric analytes is involved.

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Porous graphitic carbon chromatography–tandem mass spectrometry for the study of isoprostanes in human cerebrospinal fluid

Cited by 12 publications

References 20 publications

A new, validated HPLC‐MS/MS method for the simultaneous determination of the anti‐cancer agent capecitabine and its metabolites: 5′‐deoxy‐5‐fluorocytidine, 5′‐deoxy‐5‐fluorouridine, 5‐fluorouracil and 5‐fluorodihydrouracil, in human plasma

A new, validated HPLC‐MS/MS method for the simultaneous determination of the anti‐cancer agent capecitabine and its metabolites: 5′‐deoxy‐5‐fluorocytidine, 5′‐deoxy‐5‐fluorouridine, 5‐fluorouracil and 5‐fluorodihydrouracil, in human plasma

Fast and simple online sample preparation coupled with capillary LC‐MS/MS for determination of prostaglandins in cell culture supernatants

Utility of porous graphitic carbon stationary phase in quantitative liquid chromatography/tandem mass spectrometry bioanalysis: quantitation of diastereomers in plasma

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