Ultra-high-performance liquid chromatography for the determination of exenatide in monkey plasma by tandem quadrupole mass spectrometry

作     者：Jin-Feng Zhang Chun-Jie Sha Yu Sun Yun-Yun Gai Ji-Ye Sun Jiang-Bin Han Xin Shao Chun-Na Sha You-Xin Li Wan-Hui Liu 

作者机构：School of PharmacyYantai University State Key Laboratory of Long-acting and Targeting Drug Delivery SystemShandong Luye Pharmaceutical Co.Ltd. State Key Laboratory of Long-acting and Targeting Drug Delivery SystemShandong Luye Pharmaceutical Co. Ltd. Rushan People's Hospital 

出 版 物：《Journal of Pharmaceutical Analysis》 (药物分析学报（英文版）)

年 卷 期：2013年第3卷第4期

页      面：235-240页

学科分类：0710[理学-生物学] 1007[医学-药学(可授医学、理学学位)] 1002[医学-临床医学] 0817[工学-化学工程与技术] 0703[理学-化学] 10[医学] 0702[理学-物理学] 

基　　金：supported by the National Basic Research Program of China (973 Program) (No. 2010CB735602 and No. 2012CB724003) 

主　　题：Exenatide UPLC/MS/MS Pharmacokineties Plasma Monkey 

摘      要：A highly sensitive ultra-high-performance liquid chromatographic-tandem mass spectro- metry （UPLC/MS/MS） method was developed for the quantification of the synthetic peptide drug of exenatide in monkey plasma. Sample preparation was carried out by solid-phase extraction （SPE）, and bivalirudin was used as the internal standard （IS）. An excellent chromatographic separation was obtained on a reversed-phase C1s column with a gradient elution. Detection utilized a Qtrap 5500 system operated in the positive ion mode with multiple reaction monitoring （MRM）. The proposed method was validated by assessing the specificity, linearity, intra- and inter-day precision and accuracy, recovery, and stability. The method resulted in a linear calibration range of 0.10-30 ng/mL, extracting with only 50 μL monkey plasma aliquots. The intra- and inter-day precisions （as relative standard deviation） were less than 7.5% and 9.6%, respectively. The methodcould be successfully utilized for the pharrnacokinetic study of exenatide in monkeys following a single subcutaneous injection of Byetta.