Journal article
Reversed phase UPLC/APCI-MS determination of Vitamin K1 and menaquinone-4 in human plasma: Application to a clinical study
Journal of pharmaceutical and biomedical analysis, Vol.183, pp.113147-113147
05/10/2020
DOI: 10.1016/j.jpba.2020.113147
Abstract
•Optimized sensitive and rapid LC–MS/MS method of phylloquinone and menaquinone-4 quantification in human plasma.•The assay was linear over the concentration range from 0.01 to 50 ng/mL for both analytes.•The validated method was successfully applied to a clinical study in patients with neurodegenerative diseases.
A rapid and sensitive liquid chromatographic-tandem mass spectrometric method was developed and validated to simultaneously quantitate vitamin K1 (PK) and vitamin K2 (MK-4) concentrations in human plasma to evaluate nutritional interventions. Charcoal-stripped human plasma was used for standard and calibration preparation with vitamin E-d6 as the internal standard. Patient plasma samples were extracted using n-hexane and analytes separated using an ACE –PFP C18 column (50 × 2.1 mm, 3 μ) equipped with standard C18 guard. The mobile phase consisted of 0.1 % formic acid in water and 0.1 % formic acid in methanol at a flow rate of 0.5 mL/min. Analyte quantification was achieved by using MS/MS with a positive atmospheric pressure chemical ionization in multiple reaction monitoring (MRM) mode. The lower limit of quantification was 0.01 ng/mL for both PK and MK-4. The assay was linear over the concentration range from 0.01–50 ng/mL for all analytes with a determination coefficient (r2) of 0.998 or better. The intra-and inter-day accuracy and precision were within the acceptable limits per FDA guidance. The validated method was successfully applied to a clinical study for quantification of PK and MK-4 in human plasma to assess nutritional status and dietary interventions in patients with neurodegenerative diseases. Baseline plasma concentrations of PK and MK-4 ranged from 0.23 to 1.81 ng/mL and 0.33–0.57 ng/mL, respectively.
Details
- Title: Subtitle
- Reversed phase UPLC/APCI-MS determination of Vitamin K1 and menaquinone-4 in human plasma: Application to a clinical study
- Creators
- Yuning Zhang - Department of Pharmacy, Nanfang Hospital, Southern Medical University, Guangzhou, 510515, ChinaYashpal S Chhonker - Clinical Pharmacology Laboratory, Department of Pharmacy Practice and Science, University of Nebraska Medical Center, Omaha, NE, 68198, United StatesVeenu Bala - Clinical Pharmacology Laboratory, Department of Pharmacy Practice and Science, University of Nebraska Medical Center, Omaha, NE, 68198, United StatesAlex Hagg - University of Iowa College of Pharmacy, University of Iowa, Iowa City, IA, 52242, United StatesLinda G Snetselaar - Nutrition Center, Department of Epidemiology, College of Public Health, University of Iowa, Iowa City, IA, 52242, United StatesTerry L Wahls - Extended Care and Rehabilitation Service Line, Iowa City Veteran Affairs Health Care System, Department of Internal Medicine, Carver College of Medicine, The University of Iowa, Iowa City, IA, 52242, United StatesDaryl J Murry - Clinical Pharmacology Laboratory, Department of Pharmacy Practice and Science, University of Nebraska Medical Center, Omaha, NE, 68198, United States
- Resource Type
- Journal article
- Publication Details
- Journal of pharmaceutical and biomedical analysis, Vol.183, pp.113147-113147
- Publisher
- Elsevier B.V
- DOI
- 10.1016/j.jpba.2020.113147
- ISSN
- 0731-7085
- eISSN
- 1873-264X
- Grant note
- name: Direct-MS; name: Institute for Clinical and Translational Science at the University of Iowa; DOI: 10.13039/100000002, name: National Institutes of Health, award: U54TR001356; name: Clinical and Translational Science Award (CTSA) program
- Language
- English
- Date published
- 05/10/2020
- Academic Unit
- Holden Comprehensive Cancer Center; Neurology; General Internal Medicine; Epidemiology; Fraternal Order of Eagles Diabetes Research Center; Internal Medicine
- Record Identifier
- 9984215048902771
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