An investigation into the application of capillary electrochromatography-mass spectrometry (CEC-MS) for the analysis and quantification of a potential drug candidate in extracted plasma

Paterson, Clare J.; Boughtflower, Robert J.; Higton, David; Palmer, Elliott A.

doi:10.1007/bf02490519

Cited by 25 publications

(7 citation statements)

References 23 publications

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“…Many reports on CEC-MS have focused on the characterization of the coupling between the two techniques [155, 201±206]. CEC-MS has been used recently for several applications including analysis of samples containing, for example, peptides and amino acids [130,156,183,204], preservatives is pharmaceutical creams [127], metal ions [207], triglycerides and fatty acids [204,208], DNA [209±211], tags from combinatorial organic synthesis [212], drug candidates [213], and fatty acids and vitamins [204], among others.…”

Section: Detectionmentioning

confidence: 99%

Recent progress in capillary electrochromatography

et al. 2000

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Capillary electrochromatography (CEC) continues to captivate many separation scientists. A remarkable activity is apparent from the numerous publications in the literature using CEC. A review of the most recent progress in CEC is presented herein, covering an extensive fraction of the literature on CEC published from the year 1997 until the beginning of 2000. Most of the recent developments have concentrated on column technology.

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Section: Detectionmentioning

confidence: 99%

Recent progress in capillary electrochromatography

et al. 2000

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“…As a future development, coupling with mass spectrometry would further increase the sensitivity and selectivity [47] and therefore allow efficient screening of large libraries as obtained from combinatorial chemistry. With increased sensitivity, genetically engineered cells carrying overexpressed cellular receptors could replace particles with immobilized antibodies.…”

Section: Discussionmentioning

confidence: 99%

Immunoaffinity screening with capillary electrochromatography

et al. 2002

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Highly efficient capillary electrochromatographic separations of cardiac glycosides and other steroids are presented. Employing butyl-derivatized silica particles as stationary phase resulted in a nearly three times faster electroosmotic flow (EOF) compared to capillary electrochromatography (CEC) with octadecyl silica particles. On-column focusing with a preconcentration factor of 180 was performed and separation efficiencies of up to 240,000 plates per meter were obtained. Using label-free standard UV absorbance, detection limits of 10-80 nM were reached for all steroids tested. For screening of cardiac glycosides, e.g., digoxin and digitoxin in mixtures of steroids, CEC was combined with immunoaffinity extraction using immobilized polyclonal anti-digoxigenin antibodies and F(ab) fragments. Simply adding small amounts of antibody carrying particles to the samples and comparing chromatograms before and after antibody addition allowed screening for high affinity antigens in mixtures with moderate numbers of compounds. Under conditions of competing antigens, affinity fingerprints of immobilized anti-digoxigenin and anti-digitoxin antibodies were obtained, reflecting the cross-reactivity of eleven steroids. The method provides high selectivity due to the combination of bioaffinity interaction with highly efficient CEC separation and UV detection at several wavelengths in parallel. This selectivity was exploited for the detection of four cardiac glycosides in submicromolar concentrations in an untreated urine sample.

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“…Only a few articles have demonstrated CEC separations of plasma samples [27][28][29] 9 For the separation of corticosteroids in plasma, Taylor et al used dialysis in combination with gradient CEC for trace enrichment. Paterson et al and Stead et al reported the essential use of solid phase extraction (SPE) prior to the CEC separation of plasma samples.…”

Section: Introductionmentioning

confidence: 99%

Capillary electrochromatography of complex plasma matrix on a C18/SCX column using UV-vis and mass spectrometric detection

Spikmans

Lane²,

Smith

2000

Chromatographia

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SummarySeparations of compounds in plasma were performed on a Hypersil Duet C18/SCX capillary electrochromatography (CEC) column, utilizing an automated injection system combined with a short in-house designed and fabricated micro-electrospray CEC mass spectrometer interface. Protein precipitation was used prior to the CEC separations. More than two hundred separations of the corticosteroids Dexamethasone and Betamethasone 17-valerate, and Fluticasone Propionate in complex plasma matrix were performed on a single column under isocratic conditions. The method demonstrated good reproducibility, selectivity, sensitivity and high efficiencies. Linear calibration with good correlation was typical. Estimated detection limits in the low micromolar and nanomolar range for all compounds were obtained using UV-Vis absorbance (UV) and Electrospray Mass Spectrometric (ES/MS) detection respectively. Efficiencies for all compounds were typically 87,500 plates on a 25 cm column (350,000 plates m -1) and increased with the number of plasma samples injected, up to 250,000 plates per column (1,000,000 plates m<). These very high observed plate counts may be artificially enhanced by the inadequate scan possibilities of the MS over very narrow chromatographic peaks.

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An investigation into the application of capillary electrochromatography-mass spectrometry (CEC-MS) for the analysis and quantification of a potential drug candidate in extracted plasma

Cited by 25 publications

References 23 publications

Recent progress in capillary electrochromatography

Recent progress in capillary electrochromatography

Immunoaffinity screening with capillary electrochromatography

Capillary electrochromatography of complex plasma matrix on a C18/SCX column using UV-vis and mass spectrometric detection

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