Simultaneous determination of various cardiac glycosides by liquid chromatography–hybrid mass spectrometry for the purity assessment of the therapeutic monitored drug digoxin

Josephs, R D; Daireaux, Adeline; Westwood, Steven; Wielgosz, Robert

doi:10.1016/j.chroma.2010.04.060

Cited by 26 publications

(26 citation statements)

References 13 publications

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“…. sugar loss and dehydration of cardenolides agreed with previous reports but with higher mass resolution, allowing unambiguous assignment of precursor and product ions [8,21].…”

supporting

confidence: 88%

Profiling and structural analysis of cardenolides in two species of Digitalis using liquid chromatography coupled with high-resolution mass spectrometry

Ravi

Guardian

Dickman

et al. 2019

Preprint

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Plants of the Digitalis genus contain a cocktail of cardenolides commonly prescribed to treat heart failure. Cardenolides in Digitalis extracts have been conventionally quantified by highperformance liquid chromatography yet the lack of structural information compounded with possible co-eluents renders this method insufficient for analyzing cardenolides in plants. The goal of this work is to structurally characterize cardiac glycosides in fresh-leaf extracts using liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) that provides exact masses. Fragmentation of cardenolides is featured by sequential loss of sugar units while the steroid aglycon moieties undergo stepwise elimination of hydroxyl groups, which distinguishes different aglycones. The sequence of elution follows diginatigenin digoxigenin gitoxigenin gitaloxigenin digitoxigenin for cardenolides with the same sugar units but different aglycones using a reverse-phase column. A linear range of 0.8-500 ng g -1 has been achieved for digoxigenin, β -acetyldigoxin, and digitoxigenin with limits of detection ranging from 0.09 to 0.45 ng g -1 . A total of 17 cardenolides have been detected with lanatoside A, C, and E as major cardenolides in Digitalis lanata while 7 have been found in Digitalis purpurea including purpurea glycoside A, B, and E. Surprisingly, glucodigifucoside in D. lanata and verodoxin and digitoxigenin fucoside in D. purpurea have also been found as major cardenolides. As the first MS/MS-based method developed for analyzing cardenolides in plant extracts, this method serves as a foundation for complete identification and accurate quantification of cardiac glycosides, a necessary step towards understanding the biosynthesis of cardenolide in plants.

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“…. sugar loss and dehydration of cardenolides agreed with previous reports but with higher mass resolution, allowing unambiguous assignment of precursor and product ions [8,21].…”

supporting

confidence: 88%

Profiling and structural analysis of cardenolides in two species of Digitalis using liquid chromatography coupled with high-resolution mass spectrometry

Ravi

Guardian

Dickman

et al. 2019

Preprint

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“…Meanwhile, highly sophisticated and validated techniques like HPLC-MS allow for the reliable determination of cardenolides as well as their corresponding genins, even in the pg/g range [184]. However, the HPLC protocols introduced by Max Wichtlʼs group [6,[185][186][187] are still relevant.…”

Section: Analytical Protocolsmentioning

confidence: 99%

The Foxgloves (Digitalis) Revisited

Kreis

2017

Planta Med

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This review provides a renewed look at the genus Digitalis. Emphasis will be put on those issues that attracted the most attention or even went through paradigmatic changes since the turn of the millennium. PubMed and Google Scholar were used (“Digitalis” and “Foxglove” were the key words) to identify research from 2000 till 2017 containing data relevant enough to be presented here. Intriguing new results emerged from studies related to the phylogeny and taxonomy of the genus as well as to the biosynthesis and potential medicinal uses of the key active compounds, the cardiac glycosides. Several Eastern and Western Foxgloves were studied with respect to their propagation in vitro. In this context, molecular biology tools were applied and phytochemical analyses were conducted. Structure elucidation and analytical methods, which have experienced less exciting progress, will not be considered here in great detail.

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“…Mass fractions of the stock solutions have been calculated according to a procedure described elsewhere, [19] assuming a purity (P ANG ) of 800 mg/g with an asymmetric standard uncertainty of +100/-115 mg/g. The purity and the corresponding uncertainty of the synthetic peptide standards used for external calibrations were estimated by use of a conservative approach described in Westwood et al [18] For details about the calculation of mass fractions of peptide standard stock solutions and dilutions and their associated uncertainties, please refer to section S.1 of the Supporting Information.…”

Section: Gravimetric Preparation Of Standardsmentioning

confidence: 99%

Accurate quantification of impurities in pure peptide material – angiotensin I: Comparison of calibration requirements and method performance characteristics of liquid chromatography coupled to hybrid tandem mass spectrometry and linear ion trap high‐resolution mass spectrometry

Stoppacher

Josephs

Daireaux

et al. 2015

Rapid Comm Mass Spectrometry

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Simultaneous determination of various cardiac glycosides by liquid chromatography–hybrid mass spectrometry for the purity assessment of the therapeutic monitored drug digoxin

Cited by 26 publications

References 13 publications

Profiling and structural analysis of cardenolides in two species of Digitalis using liquid chromatography coupled with high-resolution mass spectrometry

Profiling and structural analysis of cardenolides in two species of Digitalis using liquid chromatography coupled with high-resolution mass spectrometry

The Foxgloves (Digitalis) Revisited

Accurate quantification of impurities in pure peptide material – angiotensin I: Comparison of calibration requirements and method performance characteristics of liquid chromatography coupled to hybrid tandem mass spectrometry and linear ion trap high‐resolution mass spectrometry

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