Wang Xiangyang, Yan Kaijing, Ma Xiaohui, Li Wei, Chu Yang, Guo Jiahua, Li Shuming, Zhou Shuiping, Zhu Yonghong, Liu Changxiao
Tasly Academy, Tianjin Tasly Group Co., Ltd., Tianjin, China.
Tasly Academy, Tianjin Tasly Group Co., Ltd., Tianjin, China School of Pharmaceutical Science and Technology, Tianjin University, Tianjin, China.
J Chromatogr Sci. 2016 May-Jun;54(5):697-705. doi: 10.1093/chromsci/bmv240. Epub 2016 Mar 10.
A very simple and selective high-performance liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS-MS) method was developed for simultaneous determination and pharmacokinetic study of protocatechuic aldehyde (PAL) and its active metabolite protocatechuic acid (PCA). The method involves a simple liquid-liquid extraction with ethyl acetate. The separation was performed on a Hypersil GOLD C18 column (2.1 × 150 mm, 3.0 µm; particle, Thermo, USA) with isocratic elution using a mobile phase consisted of methanol and water (containing 0.1% formic acid) at a flow rate of 0.2 mL/min. The detection of target compounds was done by using low-energy collision dissociation tandem mass spectrometry (CID-MS-MS) using the selective reaction monitoring scan mode. The method was linear for all analytes over the investigated range for all correlation coefficients greater than 0.9950. The lower limits of quantification were 2.0 ng/mL for PAL and PCA. The intra- and interday precisions (relative standard deviation, RSD %) were <6.84 and 5.54%, and the accuracy (relative error, RE %) was between -2.85 and 0.74% (n = 6). The developed method was applied to study the pharmacokinetics of PAL and its major active metabolite PCA in rat plasma after oral and intravenous administration of PAL.
建立了一种非常简单且具有选择性的高效液相色谱-电喷雾电离串联质谱法（LC-MS-MS），用于同时测定原儿茶醛（PAL）及其活性代谢产物原儿茶酸（PCA）并进行药代动力学研究。该方法采用乙酸乙酯进行简单的液-液萃取。分离在Hypersil GOLD C18柱（2.1×150 mm，3.0 µm；美国赛默飞世尔科技公司生产的填料）上进行，采用等度洗脱，流动相由甲醇和水（含0.1%甲酸）组成，流速为0.2 mL/min。目标化合物的检测采用低能量碰撞解离串联质谱法（CID-MS-MS），采用选择性反应监测扫描模式。在所有相关系数大于0.9950的研究范围内，该方法对所有分析物均呈线性。PAL和PCA的定量下限均为2.0 ng/mL。日内和日间精密度（相对标准偏差，RSD%）分别<6.84%和5.54%，准确度（相对误差，RE%）在-2.85%至0.74%之间（n = 6）。所建立的方法应用于研究大鼠口服和静脉注射PAL后血浆中PAL及其主要活性代谢产物PCA的药代动力学。
