Determination of oxyntomodulin, an anorectic polypeptide, in rat plasma using 2D-LC–MS/MS coupled with ion pair chromatography

Halquist, Matthew S.; Sakagami, Masahiro; Karnes, H. Thomas

doi:10.1016/j.jchromb.2012.06.047

Cited by 20 publications

(10 citation statements)

References 34 publications

(39 reference statements)

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“…For example, a recently described method (30 ) was able to measure glucagon in plasma with a lower limit of quantification (LLOQ) of 25 pg/mL; however, the authors acknowledged that approximately half of the healthy donor samples had endogenous glucagon concentrations below this limit. Similarly, a 2-dimensional LC-MS/MS assay was developed to measure human oxyntomodulin in rat plasma after exogenous intravenous bolus dosing with a LLOQ of 1000 pg/mL (29 ), which is likely insufficient to detect endogenous concentrations. However, by using microflow immunoaffinity (IA)-LC-MS/MS, our laboratory recently reported a method of simultaneously measuring both GLP-1 (7-36) amide and GLP-1 (9 -36) amide with a LLOQ of 0.49 pmol/L (34 ).…”

confidence: 99%

Multiplexed Quantification of Proglucagon-Derived Peptides by Immunoaffinity Enrichment and Tandem Mass Spectrometry after a Meal Tolerance Test

et al. 2016

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confidence: 99%

Multiplexed Quantification of Proglucagon-Derived Peptides by Immunoaffinity Enrichment and Tandem Mass Spectrometry after a Meal Tolerance Test

et al. 2016

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“…Solid phase extraction (SPE) is another purification technique that is employed solely or along with other purification techniques for sample clean up wherein the analyte is a smaller protein or peptide [12,[14][15][16][17]. Several mixed mode SPE cartridges, combining reversed phase stationary phase along with strong cation exchange or weak anion exchange, are commercially available for peptide analysis.…”

Section: Non-selective Protein Enrichment Techniquesmentioning

confidence: 99%

“…Stable isotope labeled amino acids are obtained by substitution of certain atoms (N,C,H) with their heavy variants. The most frequently used stable isotopes are 13 C (carbon-13), 15 N (nitrogen-15), and 2 H (deuterium). A SIL-peptide can be created by using solid-phase peptide synthesis [56,62].…”

Section: Stable Isotope Labeled Peptide Internal Standardmentioning

confidence: 99%

Internal Standards for Absolute Quantification of Large Molecules (Proteins) from Biological Matrices by LC-MS/MS

Faria¹,

Halquist²

2018

Calibration and Validation of Analytical Methods - A Sampling of Current Approaches

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Internal standardization plays a critical role in the performance of a bioanalytical method. There has been a tremendous increase in the popularity of using liquid chromatography tandem mass spectrometry (LC-MS/MS) methods for quantitative bioanalysis of protein molecules. Protein, being too large to be directly analyzed by LC-MS/MS, is proteolyzed and a characteristic peptide is used as a surrogate analyte for quantification. Internal standardization in small molecules' analysis is straightforward, i.e., either a stable labeled isotope (SIL) form of the analyte or a structural analogue is used. As protein quantification involves protein digestion to yield peptides, there are more options for internal standardization. Currently, internal standard selection is based on the availability of the internal standards and the sample preparation workflow. A SIL-form of the analyte protein is the ideal internal standard. However, its use is limited due to cost and commercial availability. Alternatively, a SIL form the surrogate peptide analyte or a cleavable SIL-peptide can be used as an IS. For preclinical bioanalysis of humanized IgG antibody-based drugs, a universal SIL analogue protein has been effectively used as an internal standard. This chapter focuses on internal standardization for the quantitative analysis of proteins, such as biotherapeutics and biomarkers, using LC-MS/MS.

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“…Case studies were discussed using m-NBA [33][34][35]. Results demonstrated at least two-to three-fold increase in sensitivity for some analytes, however, benefits are compound dependent; supercharging reagents appear to work better with large peptides.…”

Section: Key Termsmentioning

confidence: 99%

2017 White Paper on Recent Issues in Bioanalysis: Aren’t Bmv Guidance/Guidelines ‘ Scientific ’? (Part 1 – LCMS: Small Molecules, Peptides and Small Molecule Biomarkers)

Welink¹,

Yang

Hughes³

et al. 2017

Bioanalysis

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The 2017 11th Workshop on Recent Issues in Bioanalysis (11th WRIB) took place in Los Angeles/Universal City, California from 3 April 2017 to 7 April 2017 with participation of close to 750 professionals from pharmaceutical/biopharmaceutical companies, biotechnology companies, contract research organizations and regulatory agencies worldwide. WRIB was once again a 5-day, weeklong event – A Full Immersion Week of Bioanalysis, Biomarkers and Immunogenicity. As usual, it was specifically designed to facilitate sharing, reviewing, discussing and agreeing on approaches to address the most current issues of interest including both small and large molecule analysis involving LCMS, hybrid LBA/LCMS and ligand-binding assay (LBA) approaches. This 2017 White Paper encompasses recommendations emerging from the extensive discussions held during the workshop, and is aimed to provide the 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 2017 edition of this comprehensive White Paper has been divided into three parts for editorial reasons. This publication (Part 1) covers the recommendations for Small Molecules, Peptides and Small Molecule Biomarkers using LCMS. Part 2 (Biotherapeutics, Biomarkers and Immunogenicity Assays using Hybrid LBA/LCMS and Regulatory Agencies’ Inputs) and Part 3 (LBA: Immunogenicity, Biomarkers and PK Assays) are published in volume 9 of Bioanalysis, issues 23 and 24 (2017), respectively.

show abstract

Determination of oxyntomodulin, an anorectic polypeptide, in rat plasma using 2D-LC–MS/MS coupled with ion pair chromatography

Cited by 20 publications

References 34 publications

Multiplexed Quantification of Proglucagon-Derived Peptides by Immunoaffinity Enrichment and Tandem Mass Spectrometry after a Meal Tolerance Test

Multiplexed Quantification of Proglucagon-Derived Peptides by Immunoaffinity Enrichment and Tandem Mass Spectrometry after a Meal Tolerance Test

Internal Standards for Absolute Quantification of Large Molecules (Proteins) from Biological Matrices by LC-MS/MS

2017 White Paper on Recent Issues in Bioanalysis: Aren’t Bmv Guidance/Guidelines ‘ Scientific ’? (Part 1 – LCMS: Small Molecules, Peptides and Small Molecule Biomarkers)

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