Electrochemical thermospray mass spectrometry — A method for the investigation of the first steps of polymerization reactions

Hambitzer, G.; Heinz, P.P.; Stassen, I.; Heitbaum, J.

doi:10.1016/0379-6779(93)90244-q

Cited by 15 publications

(9 citation statements)

References 4 publications

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“…After assembling all parts within each block its surface was polished using a set of wet emery papers placed on a flat support. A central aperture in the Teflon spacer (3) allowed passage of the electrolyte towards the disk electrode perimeter where it converged towards the opening of the inner tube (6). The blocks were attached by 3 bolts.…”

Section: Methodsmentioning

confidence: 99%

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Radial Electrochemical Flow Cell for On‐Line Coupling with Mass Spectrometry: Theory and Electrooxidation of Dimethylaminomethyl Ferrocene

et al. 2004

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A new, radial, miniature, three-electrode flow cell is introduced. The cell×s configuration is most suitable for on-line electrochemistry ± mass spectrometry since it is characterized by low resistive losses, high conversion efficiency, and isolation of the counter electrode reaction by-products from the product stream reaching the MS. A mathematical model describing convection diffusion in the radial cell is developed. Cell×s performance can be predicted over a wide parametric range by a simple mathematical expression which converges to the Levich equation under low conversion conditions. The performance of the cell is demonstrated by studies of dimethylaminomethyl ferrocene (DMAMF) oxidation which is a simple single electron charge transfer reaction and allows validation of the mathematical model. The theoretical predictions of the model were in agreement with the results of on-line electrochemistry ± mass spectrometry studies of DMAMF.

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Section: Methodsmentioning

confidence: 99%

“…Flow rates through the flow cell were on the order of 1 mL min À1 . The cell design enabled simultaneous recording of the voltammograms and the potential dependent abundance of products and reactants of the electrochemical reaction during the potential scan [5,6].…”

Section: Introductionmentioning

confidence: 99%

Radial Electrochemical Flow Cell for On‐Line Coupling with Mass Spectrometry: Theory and Electrooxidation of Dimethylaminomethyl Ferrocene

et al. 2004

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“…Hambitzer and co-workers re-visited electrochemistry-mass spectrometry for investigation of the anodic oxidation of aniline in dilute sulfuric acid [67,68] and of N,N-dialkylanilines in neutral aqueous solution [69,70,71]. The use of a dual-beam thermospray ion source enabled the study of reactions in non-aqueous solutions.…”

Section: Redox Reactions In Additional Electrochemical Cellsmentioning

confidence: 98%

“…The use of a dual-beam thermospray ion source enabled the study of reactions in non-aqueous solutions. The arrangement was tested by elucidating the oxidation process of phenothiazine [69]. Further structural information was obtained by use of deuterated aniline [68].…”

Section: Redox Reactions In Additional Electrochemical Cellsmentioning

confidence: 99%

On-line electrochemistry – MS and related techniques

Diehl

Kärst

2002

Anal Bioanal Chem

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This review summarizes publications on the on-line coupling of electrochemistry with mass spectrometry. After a brief historic introduction it is divided into three parts, organized in order of increasing complexity of the experimental arrangement. The first section deals with the use of the electrospray ion source as an electrochemical reactor for oxidation or reduction reactions. It is followed by the second part which covers the hyphenation of different kinds of electrochemical flow cell with a variety of ionization interfaces. The last section focuses on the on-line coupling of chromatographic techniques with electrochemical flow cells and mass spectrometry.

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“…4) Getek et al utilized on-line electrochemical cell/thermospray mass spectrometry for the oxidation of acetaminophen and succeeded in detecting an oxidation product as N-acetyl-pbenzoquinoneimin, and in synthesizing acetaminophen-glutathione conjugate and acetaminophen-cysteine conjugate only by mixing the product with the corresponding thiol compound. 5) Other authors reported the electrochemical reaction of compounds by on-line electrochemistry/mass spectrometry [6][7][8][9] ; however, the electrochemical redox reaction has been rarely applied to actual studies on pharmacological metabolism using electrochemistry/thermospray tandem mass spectrometry. In recent years, the combination technique of liquid chromatography/mass spectrometry (LC-MS) has been remarkably improved and is widely available.…”

mentioning

confidence: 99%

Successful Preparation of Metabolite of Troglitazone by In-Flow Electrochemical Reaction on Coulometric Electrode

Tahara¹,

Yano²,

Kanagawa³

et al. 2007

CHEMICAL & PHARMACEUTICAL BULLETIN

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A simple, rapid and efficient system utilizing a coulometric electrode was developed for the preparation of drug metabolites. Trace amounts of reactants are usually generated in electrochemical reactions, which are not suitable for the sufficient preparation of products to obtain NMR and other spectral data for chemical structure confirmation or to obtain data from pharmacological activity screening tests of products. In the developed system, called the "in-flow electrochemical reaction system," a drug, troglitazone, was dissolved in a volatile flow solvent, and pumped into a coulometric electrode under optimized conditions, and the effluent was evaporated. Without any further purification, milligram amounts of a pure oxidation product of troglitazone could be obtained within several hours. The amount obtained was enough for 1 H-and 13 C-NMR analysis by which the structure could be confirmed and was found to be identical to one of the metabolites of troglitazone detected in human plasma. This system will be useful to prepare standard compounds of the required amount for pharmacokinetic study and for toxicokinetic study.

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Electrochemical thermospray mass spectrometry — A method for the investigation of the first steps of polymerization reactions

Cited by 15 publications

References 4 publications

Radial Electrochemical Flow Cell for On‐Line Coupling with Mass Spectrometry: Theory and Electrooxidation of Dimethylaminomethyl Ferrocene

Radial Electrochemical Flow Cell for On‐Line Coupling with Mass Spectrometry: Theory and Electrooxidation of Dimethylaminomethyl Ferrocene

On-line electrochemistry – MS and related techniques

Successful Preparation of Metabolite of Troglitazone by In-Flow Electrochemical Reaction on Coulometric Electrode

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