Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, No. 151, Malianwa North Road, Haidian District, Beijing 100193, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Jan 1;878(1):102-6. doi: 10.1016/j.jchromb.2009.11.029.
A highly sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for the determination of forsythiaside in rat plasma using epicatechin as internal standard. The analytes were extracted by solid-phase extraction and chromatographied on a C(18) column eluted with a gradient mobile phase of acetonitrile and water both containing 0.2% formic acid. The detection was performed by negative ion electrospray ionization in multiple reaction monitoring mode, monitoring the transitions m/z 623-->161 and m/z 289-->109 for forsythiaside and epicatechin, respectively. The assay was linear over the concentration ranges of 2.0-50.0 and 50.0-5000.0ng/mL with limits of detection and quantification of 0.2 and 1.0ng/mL, respectively. The precision was <10.8% and the accuracy was >91.9%, and extraction recovery ranged from 81.3% to 85.0%. This method was successfully applied to a pharmacokinetic study of forsythiaside in rats after intravenous (20mg/kg) and oral (100mg/kg) administration, and the result showed that the compound was poorly absorbed with an absolute bioavailability being approximately 0.5%.
建立了一种灵敏的液相色谱-串联质谱（LC-MS/MS）方法，用于大鼠血浆中连翘酯苷的测定，以内消旋儿茶素为内标。样品经固相萃取提取，采用含 0.2%甲酸的乙腈和水为流动相进行梯度洗脱，在负离子电喷雾电离模式下，多反应监测模式检测，用于检测连翘酯苷和内消旋儿茶素的母离子分别为 m/z 623->161 和 m/z 289->109。连翘酯苷在 2.0-50.0 和 50.0-5000.0ng/mL 浓度范围内线性良好，检测限和定量限分别为 0.2 和 1.0ng/mL。精密度<10.8%，准确度>91.9%，提取回收率为 81.3%-85.0%。该方法成功应用于大鼠静脉（20mg/kg）和口服（100mg/kg）给予连翘酯苷后的药代动力学研究，结果表明该化合物吸收较差，绝对生物利用度约为 0.5%。
