The purpose of the study is to develop an ultra performance liquid chromatographytandem mass spectrometry(UPLCeMS/MS)to determinate the concentration of azilsartan in the dog plasma.After precipitated by methanol,the ...The purpose of the study is to develop an ultra performance liquid chromatographytandem mass spectrometry(UPLCeMS/MS)to determinate the concentration of azilsartan in the dog plasma.After precipitated by methanol,the plasma sample containing azilsartan and diazepam(internal standard,IS)was determined by UPLCeMS/MS.The mobile phase consisted of acetonitrile-water was pumped at a flow rate of 0.3 ml/min in gradient elution.Kinetex 2.6 m XB-C18 column(502.1 mm,100Å;Phenomenex,USA)were used for LC separations.The column temperature was 30℃ and the injection volume was 5 ml.The electrospray ionization(ESI)and multiple reaction monitoring(MRM)were applied at the transitions of m/z 457/279(azilsartan)and m/z 285/193(diazepam),respectively.The developed method was identified a good linearity over a concentration range of 2.5e5000 ng/ml.The lower limit of quantitation(LLOQ)was 2.5 ng/ml.The intraday and inter-day precision(relative standard deviation,RSD%)were less than 10%and accuracy(relative error,RE%)was less than 5%at three quality control levels.The extraction recovery of azilsartan at three quality control levels were 82.41±0.68%,98.66±11.00%,102.43±0.82%.And the recovery for IS(100 ng/ml)was 91.75±0.54%.A validated UPLCeMS/MS method was firstly developed for the quantification of azilsartan in dog plasma and it was applied to the pharmacokinetics study.展开更多
文摘The purpose of the study is to develop an ultra performance liquid chromatographytandem mass spectrometry(UPLCeMS/MS)to determinate the concentration of azilsartan in the dog plasma.After precipitated by methanol,the plasma sample containing azilsartan and diazepam(internal standard,IS)was determined by UPLCeMS/MS.The mobile phase consisted of acetonitrile-water was pumped at a flow rate of 0.3 ml/min in gradient elution.Kinetex 2.6 m XB-C18 column(502.1 mm,100Å;Phenomenex,USA)were used for LC separations.The column temperature was 30℃ and the injection volume was 5 ml.The electrospray ionization(ESI)and multiple reaction monitoring(MRM)were applied at the transitions of m/z 457/279(azilsartan)and m/z 285/193(diazepam),respectively.The developed method was identified a good linearity over a concentration range of 2.5e5000 ng/ml.The lower limit of quantitation(LLOQ)was 2.5 ng/ml.The intraday and inter-day precision(relative standard deviation,RSD%)were less than 10%and accuracy(relative error,RE%)was less than 5%at three quality control levels.The extraction recovery of azilsartan at three quality control levels were 82.41±0.68%,98.66±11.00%,102.43±0.82%.And the recovery for IS(100 ng/ml)was 91.75±0.54%.A validated UPLCeMS/MS method was firstly developed for the quantification of azilsartan in dog plasma and it was applied to the pharmacokinetics study.
