Wang Xinyu, Pang Jihai, Newman Robert A, Kerwin Sean M, Bowman Phillip D, Stavchansky Salomon
Pharmaceutics Division, College of Pharmacy, University of Texas at Austin, Austin, TX 78712, United States.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 May 1;867(1):138-43. doi: 10.1016/j.jchromb.2008.02.025. Epub 2008 Mar 6.
The quantitative determination of caffeic acid phenethyl ester (CAPE) and its fluorinated derivative (FCAPE) from rat plasma using ultra-performance liquid chromatography with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) is reported. CAPE and FCAPE were extracted using ethyl acetate in the presence of methyl caffeate (MC) as internal standard. Separation was achieved using a C(18) column (2.1 mm x 50 mm, 1.7 microm) and gradient elution with water and acetonitrile containing 0.2% and 0.1% formic acid, respectively. A non-linear response over a broad concentration range (1-1000 ng/ml, r(2)>0.995 using a quadratic regression model and 1/concentration weighting) was obtained. The inter-day and intra-day variability for CAPE and FCAPE were found to be less than 14.2% and 9.5%, respectively. Data are presented to illustrate the practicality of the method for the pharmacokinetic evaluation of CAPE and FCAPE after intravenous administration to rats.
报道了使用超高效液相色谱-电喷雾电离串联质谱法(UPLC-ESI-MS/MS)对大鼠血浆中咖啡酸苯乙酯(CAPE)及其氟化衍生物(FCAPE)进行定量测定的方法。以咖啡酸甲酯(MC)作为内标,用乙酸乙酯从大鼠血浆中提取CAPE和FCAPE。采用C(18)柱(2.1 mm×50 mm,1.7μm),分别以含0.2%和0.1%甲酸的水和乙腈进行梯度洗脱,实现分离。在较宽的浓度范围(1 - 1000 ng/ml)内获得了非线性响应(使用二次回归模型和1/浓度加权,r(2)>0.995)。发现CAPE和FCAPE的日间和日内变异分别小于14.2%和9.5%。文中给出的数据说明了该方法在大鼠静脉注射CAPE和FCAPE后进行药代动力学评估的实用性。