Mass spectrometric recommendations for Quan/Qual analysis using liquid-chromatography coupled to quadrupole time-of-flight mass spectrometry

Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Groß, Gerhard; Vreeken, Rob J.; Hankemeier, Thomas

doi:10.1016/j.aca.2018.02.055

Cited by 17 publications

(11 citation statements)

References 19 publications

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“…22 In non-regulatory environments, a CV of 20–25% is a commonly used target. 23 The variation may have been introduced during high-throughput sample preparation, particularly during hydrolysis or during HRAM MS analysis.…”

Section: Resultsmentioning

confidence: 99%

High-throughput quantification of carboxymethyl lysine in serum and plasma using high-resolution accurate mass Orbitrap mass spectrometry

et al. 2019

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Background Carboxymethyl lysine is an advanced glycation end product of interest as a potential biomarker of cardiovascular and other diseases. Available methods involve ELISA, with potential interference, or isotope dilution mass spectrometry (IDMS), with low-throughput sample preparation. Methods A high-throughput sample preparation method based on 96-well plates was developed. Protein-bound carboxymethyl lysine and lysine were quantified by IDMS using reversed phase chromatography coupled to a high-resolution accurate mass Orbitrap Exactive mass spectrometer. The carboxymethyl lysine concentration (normalized to lysine concentration) was measured in 1714 plasma samples from the British Regional Heart Study (BRHS). Results For carboxymethyl lysine, the lower limit of quantification (LLOQ) was estimated at 0.16 μM and the assay was linear between 0.25 and 10 μM. For lysine, the LLOQ was estimated at 3.79 mM, and the assay was linear between 2.5 and 100 mM. The intra-assay coefficient of variation was 17.2% for carboxymethyl lysine, 9.3% for lysine and 10.5% for normalized carboxymethyl lysine. The inter-assay coefficient of variation was 18.1% for carboxymethyl lysine, 14.8 for lysine and 16.2% for normalized carboxymethyl lysine. The median and inter-quartile range of all study samples in each batch were monitored. A mean carboxymethyl lysine concentration of 2.7 μM (IQR 2.0–3.2 μM, range 0.2–17.4 μM) and a mean normalized carboxymethyl lysine concentration of 69 μM/M lysine (IQR 54–76 μM/M, range 19–453 μM/M) were measured in the BRHS. Conclusion This high-throughput sample preparation method makes it possible to analyse large cohorts required to determine the potential of carboxymethyl lysine as a biomarker.

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Section: Resultsmentioning

confidence: 99%

High-throughput quantification of carboxymethyl lysine in serum and plasma using high-resolution accurate mass Orbitrap mass spectrometry

et al. 2019

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“…The improved performance of HRMS systems has triggered more bioanalysts to switch from triple quadrupole MS to HRMS for quantitative analysis when additional selectivity was required [56][57][58]. There was consensus that the conclusions reached in the 2015 White Paper in Bioanalysis, i.e., HRMS technology is fit for use in regulated bioanalysis for PK and biomarker assays [10] are still valid, and there have been regulatory submissions already.…”

Section: Hrms: Small Molecule Methods Development Strategiesmentioning

confidence: 99%

2020 White Paper on Recent Issues in Bioanalysis: BMV of Hybrid Assays, Acoustic MS, HRMS, Data Integrity, Endogenous Compounds, Microsampling and Microbiome ( Part 1 –Recommendations on Industry/Regulators Consensus on BMV of Biotherapeutics by LCMS, Advanced Application in Hybrid Assays, Regulatory Challenges in Mass Spec, Innovation in Small Molecules, Peptides and Oligos)

et al. 2021

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The 14th edition of the Workshop on Recent Issues in Bioanalysis (14th WRIB) was held virtually on June 15–29, 2020 with an attendance of over 1000 representatives from pharmaceutical/biopharmaceutical companies, biotechnology companies, contract research organizations, and regulatory agencies worldwide. The 14th WRIB included three Main Workshops, seven Specialized Workshops that together spanned 11 days in order to allow exhaustive and thorough coverage of all major issues in bioanalysis, biomarkers, immunogenicity, gene therapy, cell therapy and vaccine. Moreover, a comprehensive vaccine assays track; an enhanced cytometry track and updated Industry/Regulators consensus on BMV of biotherapeutics by Mass Spectrometry (hybrid assays, LCMS and HRMS) were special features in 2020. As in previous years, this year's WRIB continued to gather a wide diversity of international industry opinion leaders and regulatory authority experts working on both small and large molecules to facilitate sharing and discussions focused on improving quality, increasing regulatory compliance and achieving scientific excellence on bioanalytical issues. This 2020 White Paper encompasses recommendations emerging from the extensive discussions held during the workshop and is aimed to provide the Global Bioanalytical Community with key information and practical solutions on topics and issues addressed, in an effort to enable advances in scientific excellence, improved quality and better regulatory compliance. Due to its length, the 2020 edition of this comprehensive White Paper has been divided into three parts for editorial reasons. This publication covers the recommendations on (Part 1) Hybrid Assays, Innovation in Small Molecules, & Regulated Bioanalysis. Part 2A (BAV, PK LBA, Flow Cytometry Validation and Cytometry Innovation), Part 2B (Regulatory Input) and Part 3 (Vaccine, Gene/Cell Therapy, NAb Harmonization and Immunogenicity) are published in volume 13 of Bioanalysis, issues 5, and 6 (2021), respectively.

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“…Each by-product was identified based on mass value (m/z) and retention times. Quantification was carried out using the TOF mode by extracting the narrow window extracted ion chromatogram (nwXIC) of the molecular ion for each compound (typically extracted using a 20 mDa window) compared with previous studies that used 20 and 50 mDa windows [27,28].…”

Section: Solid Phase Extraction (Spe) Methodsmentioning

confidence: 99%

Electrochemical Degradation of Metoprolol Using Graphite-PVC Composite as Anode: Elucidation and Characterization of New by-products Using LC-TOF/MS

et al. 2020

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Abstract. Metoprolol (MTP) is one of pharmaceuticals used for treatment of heart failure and hypertension. It was frequently detected in wastewater samples either influent or effluent. The application of graphite-PVC composite as anode was investigated for the degradation of metoprolol in the presence of strong electrolyte such as sodium chloride (NaCl). The degradation rate was strongly influenced by initial concentrations of metoprolol, NaCl concentration and applied voltage. An initial concentration of 2 mg/L was eliminated more than 95% after 30 min under optimum conditions; 5000 mg/L NaCl and 5 V. The consumption energy of the electrochemical reaction was 0.665 Wh/mg for metoprolol after 30 min. The kinetic rate constant of metoprolol could be ranged between 0.0016 and 0.0801 min-1. The electrochemical degradation efficiency of metoprolol and its by-products has been achieved. The degradation of metoprolol produced four transformated products as investigated and elucidated using liquid chromatography-time of flight/mass spectrometry. The proposed degradation pathway of metoprolol was schemed on the base of the identified intermediates. Resumen. El metoprolol (MTP) es uno de los fármacos utilizados para el tratamiento de la insuficiencia cardíaca y la hipertensión. Se detecta frecuentemente en muestras de aguas residuales, ya sea de afluentes o efluentes. Se investigó la aplicación del compuesto de grafito-PVC como ánodo para la degradación del metoprolol en presencia de un electrolito fuerte como el cloruro de sodio (NaCl). La velocidad de degradación depende de las concentraciones iniciales de metoprolol, la concentración de NaCl y el voltaje aplicado. Una concentración inicial de 2 mg/L de MTP fue eliminada con más del 95% después de 30 minutos en condiciones óptimas; 5000 mg/L de NaCl y 5 V. La energía de consumo de la reacción electroquímica fue de 0,665 Wh/mg para el metoprolol después de 30 min. La constante cinética de degradación metoprolol oscila entre 0.0016 y 0.0801 min-1. Se logró la eficiente degradación electroquímica del metoprolol y sus subproductos, ya que se detectaron cuatro subproductos electrogenerados según los resultados de cromatografía líquida - tiempo de vuelo/espectrometría de masas. La vía de degradación propuesta del metoprolol se esquematizó sobre la base de los productos intermedios identificados.

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Mass spectrometric recommendations for Quan/Qual analysis using liquid-chromatography coupled to quadrupole time-of-flight mass spectrometry

Cited by 17 publications

References 19 publications

High-throughput quantification of carboxymethyl lysine in serum and plasma using high-resolution accurate mass Orbitrap mass spectrometry

High-throughput quantification of carboxymethyl lysine in serum and plasma using high-resolution accurate mass Orbitrap mass spectrometry

Electrochemical Degradation of Metoprolol Using Graphite-PVC Composite as Anode: Elucidation and Characterization of New by-products Using LC-TOF/MS

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