A sensitive method for digoxin determination using formate-adduct ion based on the effect of ionization enhancement in liquid chromatograph–mass spectrometer

Li, Xia; Wang, Yu; Zhou, Qing-Yuan; Yu, Yunqiu; Zheng, Jie

doi:10.1016/j.jchromb.2014.11.023

Cited by 14 publications

(13 citation statements)

References 16 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The MS parameters were optimized by infusing a standard solution of analytes. The generated ions of digoxin include the positive ions [M + H] + , [M + Na] + 4,7,16 [M+ NH 4 ] + , 8,11,13,15 [M + Li] + 9 and the negative ions [M‐H] − , [M + HCOO] – , 14 [M + CF 3 COO] – 6 . However, the full MS‐SIM indicated that the presence of the formic acid gave rise to formate‐adduct ions [M + HCOO] − as the predominant ion for digoxin, with an m/z value of 825.42781.…”

Section: Resultsmentioning

confidence: 99%

“…The choice of online‐SPE cartridge was the critical step because it could significantly influence the analyte recovery and matrix effects. Among the reported offline SPE pretreatment methods for digoxin, the use of an Oasis HLB cartridge mostly gave recoveries near 100% 10,11,13,14 . We therefore adopted the corresponding online HLB cartridge for pretreatment, and a 100% water wash over 2 min was sufficient to remove matrix 23 .…”

Section: Resultsmentioning

confidence: 99%

“…Among the reported offline SPE pretreatment methods for digoxin, the use of an Oasis HLB cartridge mostly gave recoveries near 100%. 10,11,13,14 We therefore adopted the corresponding online HLB cartridge for pretreatment, and a 100% water wash over 2 min was sufficient to remove matrix. 23 This cartridge also exhibited satisfactory elution of digoxin, and an eluent of ACN/formic acid A/B (30/70) over 1 min was sufficient to elute the analytes to the analytical column.…”

Section: Online-spe-lc Optimizationmentioning

confidence: 99%

“…In the past decade, determination of digoxin in biological specimens was primarily accomplished using liquid chromatography tandem mass spectrometry (LC-MS, LC-MS/MS) 4,[6][7][8][9][10][11][12][13][14][15] and surfaceassisted laser desorption/ionization mass spectrometric detection (SALDI/MS). 16 MS/MS offered considerable advantages, including speed, selectivity, sensitivity, and robustness, and was a highly efficient analytical tool for biological specimens.…”

Section: Introductionmentioning

confidence: 99%

“…17 Recent developments in high-resolution mass spectrometry (HRMS) had resulted in quantitation abilities comparable to those of MS/MS, besides its high resolving power, high mass accuracy, and highperformance quadrupole for selectivity. 18,19 Sample pretreatment methods prior to the analytical procedure were similar across methods, such as liquid-liquid extraction (LLE), [6][7][8] protein precipitation (PP), 4,9,12,15 and solid-phase extraction (SPE) 10,11,13,14 as well as dispersive liquid-liquid microextraction. 16 These traditional techniques are time-consuming and labor-intensive especially for a large number of samples.…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

An automated streamlined method for the therapeutic drug monitoring of digoxin based on the online‐solid‐phase extraction liquid chromatography tandem high‐resolution mass spectrometry

Liu

Wang

Pan

et al. 2021

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

Rationale Digoxin is widely used in the clinical treatment of cardiovascular diseases. However, due to its extremely narrow therapeutic window, therapeutic drug monitoring (TDM) is vitally important. In consideration of the time‐consuming and labor‐intensive nature of the traditional techniques, an automated and efficient method was required for the clinical individualized TDM of digoxin. Methods An online solid‐phase extraction liquid chromatography tandem high‐resolution mass spectrometry (online‐SPE‐LC‐HRMS) method was developed and applied for the determination of digoxin in plasma. The online SPE‐LC steps included pretreatment and separation of plasma samples that were carried out using a Waters Oasis HLB cartridge and XBridge Shield RP18 column, respectively. A high‐resolution Q Orbitrap mass spectrometer with targeted‐selected ion monitoring in negative scan mode was applied to monitor formate‐adduct ions [M + HCOO]− m/z 825.42781 for digoxin. Results Linearity was shown over the range 0.1–10 ng mL−1 for digoxin with correlation coefficients of R2 > 0.999. The lower limit of quantitation (LLOQ) for digoxin was 0.1 ng mL−1. Extraction recoveries ranged from 82.61% to 94.28% for digoxin. The intra‐ and inter‐day precision values were < 5.53% with accuracy ranging from 84.97% to 96.75%. The total running time was 10 min for each sample. Conclusion The established method displayed satisfactory recoveries, accuracy, precision, and stability, and successfully applied on the TDM of digoxin. This automated streamlined method provides a powerful tool to guide the individualized administration of digoxin, which is significant for the practice of precision medicine.

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Online-spe-lc Optimizationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

An automated streamlined method for the therapeutic drug monitoring of digoxin based on the online‐solid‐phase extraction liquid chromatography tandem high‐resolution mass spectrometry

Liu

Wang

Pan

et al. 2021

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

show abstract

Development of a new ultra‐high‐performance liquid chromatography–tandem mass spectrometry method for the determination of digoxin and digitoxin in plasma: Comparison with a clinical immunoassay

et al. 2022

View full text Add to dashboard Cite

Cardiac glycosides digoxin and digitoxin are used in therapy for the treatment of congestive heart failure. Moreover, these compounds can be responsible for intoxication cases caused by fortuitous ingestion of leaves of Digitalis. Due to the narrow therapeutic range of these drugs, therapeutic drug monitoring is recommended in the clinical practice. In this context, immunoassays‐based methods are generally employed but digoxin‐ and digitoxin‐like compounds can interfere with the analysis. The aim of this study was to develop and validate an original UPLC–MS/MS method for the determination of digoxin and digitoxin in plasma. The method shows adequate sensitivity and selectivity with acceptable matrix effects and very good linearity, accuracy, precision, and recovery. A simple liquid–liquid extraction procedure was used for sample clean‐up. The method was applied for the analysis of n = 220 plasma samples collected in two different clinical chemistry laboratories and previously tested by the same immunoassay. The statistical comparison showed a relevant negative bias of the UPLC–MS/MS method versus the immunoassay. These results are consistent with an immunoassay overestimation of digoxin plasmatic levels due to cross‐reaction events with endogenous digoxin‐like substances.

show abstract

Mass Spectrometry‐based Personalized Drug Therapy

Cui

Wang

Tan

et al. 2020

Mass Spectrometry Reviews

View full text Add to dashboard Cite

Personalized drug therapy aims to provide tailored treatment for individual patient. Mass spectrometry (MS) is revolutionarily involved in this area because MS is a rapid, customizable, cost‐effective, and easy to be used high‐throughput method with high sensitivity, specificity, and accuracy. It is driving the formation of a new field, MS‐based personalized drug therapy, which currently mainly includes five subfields: therapeutic drug monitoring (TDM), pharmacogenomics (PGx), pharmacomicrobiomics, pharmacoepigenomics, and immunopeptidomics. Gas chromatography‐MS (GC‐MS) and liquid chromatography‐MS (LC‐MS) are considered as the gold standard for TDM, which can be used to optimize drug dosage. Matrix‐assisted laser desorption ionization‐time of flight‐MS (MALDI‐TOF‐MS) significantly improves the capability of detecting biomacromolecule, and largely promotes the application of MS in PGx. It is becoming an indispensable tool for genotyping, which is used to discover and validate genetic biomarkers. In addition, MALDI‐TOF‐MS also plays important roles in identity of human microbiome whose diversity can explain interindividual differences of drug response. Pharmacoepigenetics is to study the role of epigenetic factors in individualized drug treatment. MS can be used to discover and validate pharmacoepigenetic markers (DNA methylation, histone modification, and noncoding RNA). For the emerging cancer immunotherapy, personalized cancer vaccine has effective immunotherapeutic activity in the clinic. MS‐based immunopeptidomics can effectively discover and screen neoantigens. This article systematically reviewed MS‐based personalized drug therapy in the above mentioned five subfields. © 2020 John Wiley & Sons Ltd. Mass Spec Rev

show abstract

A sensitive method for digoxin determination using formate-adduct ion based on the effect of ionization enhancement in liquid chromatograph–mass spectrometer

Cited by 14 publications

References 16 publications

An automated streamlined method for the therapeutic drug monitoring of digoxin based on the online‐solid‐phase extraction liquid chromatography tandem high‐resolution mass spectrometry

An automated streamlined method for the therapeutic drug monitoring of digoxin based on the online‐solid‐phase extraction liquid chromatography tandem high‐resolution mass spectrometry

Development of a new ultra‐high‐performance liquid chromatography–tandem mass spectrometry method for the determination of digoxin and digitoxin in plasma: Comparison with a clinical immunoassay

Mass Spectrometry‐based Personalized Drug Therapy

Contact Info

Product

Resources

About