Determination of flomoxef in human plasma by liquid chromatography/electrospray ionization tandem mass spectrometry

被引:0
|
作者
Kravtsova, Oxana Yu. [1 ]
Paramonov, Sergey A. [1 ]
Vasilevich, Natalya I. [1 ]
Kazyulkin, Denis N. [1 ]
Vlasova, Ekaterina [2 ]
Engsig, Michael [2 ]
机构
[1] Bioscreening Lab Co Ltd, Moscow 125480, Russia
[2] Nycomed, Russian Innovat Ctr, Moscow 119048, Russia
关键词
flomoxef; human plasma; LC-MS; MS analysis; tandem mass-spectrometry; ANTIBIOTICS;
D O I
10.1002/bmc.2968
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A specific, sensitive, rapid and reproducible method for the determination of flomoxef in human plasma using high-performance liquid chromatography-tandem mass spectrometry was developed and validated. Flomoxef was detected using an electrospay ionization method operated in negative-ion mode. Chromatographic separation was performed in gradient elution mode on a Luna (R) C-18(2) column (3 m, 20 x 4.0 mm) at a flow rate of 1 mL/min and runtime 3.5 min. The mobile phase consisted of acetonitrile and water containing 0.1% formic acid as additive. Extraction of flomoxef from plasma and precipitation of plasma proteins was performed with acetonitrile with an absolute recovery of 86.4 +/- 1.6%. The calibration curve was linear with a correlation coefficient of 0.999 over the concentration range 10-5000 ng/mL and the lower limit of quantification was 10 ng/mL. The intra- and inter-day precisions were <11.8%, while the accuracy ranged from 99.6 to 109.0%. A stability study of flomoxef revealed that it could be successfully analyzed at 4oC over 24 h, but it was unstable in solutions at room temperature during short-term storage (4 h) and several freeze-thaw cycles. Copyright (c) 2013 John Wiley & Sons, Ltd.
引用
收藏
页码:1609 / 1614
页数:6
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