Determination of eptifibatide concentration in human urine utilizing the liquid chromatography-tandem mass spectrometry method
A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed for the determination of eptifibatide in human urine.Following protein precipitation,analytes were separated on an Agilent ZORBAX Eclipse XDB-C18 column with the mobile phase consisted of methanol-0.008 mol/L ammonium formate in water (containing 0.1% formic acid) (35 ∶ 65).A tandem mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode.Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 832.6-159.4 and 931.6-745.6 for eptifibatide and internal standard,respectively.The method showed a good linearity in a concentration range of 5-5000 ng/mL for eptifibatide with the LLOQ of 5ng/mL.Matrix effects,for eptifibatide at three concentrations of 10,200 and 4000 ng/mL and for IS at one concentration of 267 ng/mL,were found to be 99%,92%,96%,and 109%,respectively.At three QC concentration levels 10,200 and 4000ng/mL,the percent extraction recoveries of eptifibatide obtained from urine were 96%、98% and 93%,respectively.The mean recovery for the internal standard EPM-05 at the concentration employed was 107%.Eptifibatide in human urine showed good stability with founded concentrations ranged from 90.2-108.2% of the initials.
eptifibatide liquid chromatography-tandem mass spectrometry urine drug concentration urineexcretion rate
ZHOU Zhi-ling CHEN Xiu-yun LIN Shu-guang YU Xi-yong YANG Min SHAN Zhi-xin LIN Qiu-xiong MAI Li-ping DENG Chun-yu ZHANG Meng-zhen CHEN Tie-feng LIU Xiao-ying
Medical Research Center of Guangdong General Hospital, Guangdong Provincial Cardiovascular Institute,Guangdong Academy of Medical Sciences, Guangzhou 510080, China
国内会议
成都
英文
351-351
2012-10-26（万方平台首次上网日期，不代表论文的发表时间）