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Quantitative determination of plasma vitamin K1 by high-performance liquid chromatography coupled to isotope dilution tandem mass spectrometry.

Abstract
Plasma vitamin K1 (phylloquinone) determination is commonly used for the diagnosis of vitamin K deficiency in patients suffering from lipid malabsorption. Moreover, current evidence that adequate vitamin K intake, and correspondingly adequate plasma vitamin K1 concentration, could also be of importance in relation to bone and brain diseases emphasizes the need to improve the current analytical methods. We developed a liquid chromatography coupled to tandem mass spectrometry method using a stable isotope ring-D4-labeled internal standard of vitamin K1 and operating in the multiple reaction monitoring mode by the selection of a precursor and product ions. The atmospheric pressure chemical ionization (APCI) method was shown to be more sensitive than electrospray ionization. After a single-step extraction with cyclohexane, chromatographic separation was performed on a C18 column with an isocratic mobile phase. The linearity was up to 5400ng/L, and the limit of detection was 14ng/L. Intra- and interrun precision were 2.4% and 8.3%, respectively, for the lower limit of the reference range. Recovery was better than 98%. The method is simple and reliable, allowing accurate vitamin K1 measurement in plasma samples from healthy subjects and patients suffering from vitamin K deficiency.
AuthorsVéronique Ducros, Mickaël Pollicand, François Laporte, Alain Favier
JournalAnalytical biochemistry (Anal Biochem) Vol. 401 Issue 1 Pg. 7-14 (Jun 01 2010) ISSN: 1096-0309 [Electronic] United States
PMID20175981 (Publication Type: Journal Article)
CopyrightCopyright 2010 Elsevier Inc. All rights reserved.
Chemical References
  • Cyclohexanes
  • Cyclohexane
  • Vitamin K 1
Topics
  • Chromatography, High Pressure Liquid (methods)
  • Cyclohexanes (chemistry)
  • Humans
  • Isotope Labeling
  • Tandem Mass Spectrometry (methods)
  • Vitamin K 1 (blood, isolation & purification)
  • Vitamin K Deficiency (diagnosis)

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