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

被引:41
作者
Ducros, Veronique [1 ]
Pollicand, Mickael [1 ]
Laporte, Francois [1 ]
Favier, Alain [1 ]
机构
[1] CHU Grenoble, Dept Biol Integree, F-38043 Grenoble, France
关键词
Vitamin K1; Phylloquinone; Tandem mass spectrometry; Clinical sample; PHYLLOQUINONE; SERUM; HPLC; REDUCTION; PROTEINS; ASSAY;
D O I
10.1016/j.ab.2010.02.018
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 5400 ng/L, and the limit of detection was 14 ng/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. (C) 2010 Elsevier Inc. All rights reserved.
引用
收藏
页码:7 / 14
页数:8
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