FIELD: chemistry.
SUBSTANCE: calibration solutions of warfarin alcohol with concentration of 0, 10, 25, 50, 75, 100 ng/ml are prepared. Analysed samples are then prepared and analysed on a mass-spectrometer in negative ion detection mode with the following analysis parameters: aliquot volume - 50 mcl, eluent flow rate- 0.8-1.0 ml/min, mobile phase - 50% acetonitrile, analysis time - 1-2 min, measurement range - 100-1000 m/z. Further, calibration solutions are used to plot a calibration curve based on the ratio of the peak area of ion density of warfarin alcohol to concentration of the calibration solution and concentration of warfarin alcohol in the sample is determined using the calibration curve based on peak area of ion density with 309.2 m/z determined in the sample. Blood plasma obtained 1-96 hours after taking in the last dose of warfarin is used; the mass-spectrometer used is mass-spectrometer Agilent 6410 QQQ (Agilent Technologies) with Masshunter software system; measurement accuracy is determined during analysis based on the calibration solutions used.
EFFECT: faster, more accurate and more reliable determination of concentration of warfarin alcohol in blood plasma.
6 cl, 5 dwg, 1 tbl, 2 ex
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Authors
Dates
2013-06-27—Published
2012-04-25—Filed