Determination of melagatran, a novel, direct thrombin inhibitor, in human plasma and urine by liquid chromatography-mass spectrometry

被引：46

作者：

Larsson, M ^{[1
]}

Logren, U ^{[1
]}

Ahnoff, M ^{[1
]}

Lindmark, B ^{[1
]}

Abrahamsson, P ^{[1
]}

Svennberg, H ^{[1
]}

Persson, BA ^{[1
]}

机构：

[1] AstraZeneca R&D Molndal, DMPK & Bioanalyt Chem, S-43183 Molndal, Sweden

来源：

JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2002年 / 766卷 / 01期

关键词：

melagatran; thrombin;

D O I：

10.1016/S0378-4347(01)00429-7

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Analytical methods for the determination of melagatran (H 319/68) in biological samples by liquid chromatography (LC)-positive electrospray ionization mass spectrometry using multiple reaction monitoring are described. Melagatran in plasma was isolated by solid-phase extraction on octylsilica, either in separate extraction tubes or in 96-well plates. Absolute recovery of melagatran from plasma was >92%. Melagatran and the internal standard, H 319/68 D-2 C-13(2), were separated from other sample components by LC utilizing a C-18 stationary phase and a mobile phase comprising 35% acetonitrile and 0.08% formic acid in 0.0013 mol/l ammonium acetate solution. After dilution, urine was injected directly onto the LC column and subjected to gradient LC. The relative standard deviation was 1-5% for concentrations above the limit of quantification, which was estimated for plasma at 10 or 25 nmol/l for sample volumes of 500 or 200 mul, respectively, and 100 nmol/l for urine. (C) 2002 Elsevier Science B.V. All rights reserved.

引用

页码：47 / 55

页数：9