Method for the Determination of Vitamin K Homologues in Human Plasma Using High-Performance Liquid Chromatography-Tandem Mass Spectrometry

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• 作者：Yoshitomo Suhara ; Maya Kamao ; Naoko Tsugawa ; and Toshio Okano
• 刊名：Analytical Chemistry
• 出版年：2005
• 出版时间：February 1, 2005
• 年：2005
• 卷：77
• 期：3
• 页码：757 - 763
• 全文大小：301K
• 年卷期：v.77,no.3(February 1, 2005)
• ISSN：1520-6882

文摘

We report here the development of a precise and sensitivemethod for the determination of vitamin K homologuesincluding phylloquinone (PK), menaquinone-4 (MK-4),and menaquinone-7 (MK-7) in human plasma usingHPLC-tandem mass-mass spectrometry with atmosphericpressure chemical ionization (LC-APCI-MS/MS). Themethod involves the use of stable isotope ¹⁸O-labeledinternal standard compounds, which were synthesized inour laboratory, and the selection of a precursor andproduct ion with a MS/MS multiple reaction monitoringmethod. The average intraassay and interassay variationvalues for PK, MK-4, and MK-7 were <10%. Averagespiked recoveries from authentic compounds added tonormal human plasma samples for PK, MK-4, and MK-7were 98-102%. Mean plasma concentrations of PK, MK-4, and MK-7 from healthy subjects (n = 20) were 1.22 ±0.57, 0.39 ± 0.46, and 6.37 ± 7.45 ng/mL, respectively.We conclude that this novel LC-APCI-MS/MS methodshould be useful for the evaluation of vitamin K status inpostmenopausal women and elderly subjects and providesuseful information for the treatment and prevention ofosteoporosis with vitamin K.