Determination of ecabet in human plasma by high-performance liquid chromatography-tandem mass spectrometry.
This paper describes a simple, robust and cost-effective assay for the determination of ecabet in human plasma. After a simple step of protein precipitation using methanol, plasma samples were analyzed by reverse phase high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) with valsartan as the internal standard (I.S.). Ecabet and the I.S. valsartan were separated on a Venusil MP C18 analytical column using methanol-10mM ammonium acetate (75:25, v/v, pH 3.0) as mobile phase at a flow rate of 1.0 mL/min. Ecabet and I.S. were eluted at 0.91 and 0.92 min, respectively, ionized in negative mode, and then detected by multiple reaction monitoring (MRM) essay. The MRM transitions of m/z 379.1-->m/z 277.1 and m/z 434.3-->m/z 350.1 were used to quantify ecabet and I.S., respectively. The assay was linear over the concentration range of 10-6000 ng/mL and was successfully applied to a pharmacokinetic study in healthy volunteers.
Zhang
Dan
D
Research Center for Drug Metabolism, Jilin University, Changchun 130023, PR China.
Du
Xiaolin
X
Liu
Mingyuan
M
Li
Hao
H
Jiang
Yao
Y
Zhao
Limei
L
Gu
Jingkai
J
D045784:Abietanes / Q000097:blood* / Q000737:chemistry; D019540:Area Under Curve; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D006801:Humans; D057927:Hydrophobic and Hydrophilic Interactions; D000432:Methanol / Q000737:chemistry; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013777:Tetrazoles / Q000097:blood / Q000737:chemistry; D014633:Valine / Q000031:analogs & derivatives / Q000097:blood / Q000737:chemistry; D000068756:Valsartan
D045784:Abietanes; D013777:Tetrazoles; C061681:ecabet; D000068756:Valsartan; D014633:Valine; D000432:Methanol