Zan Bin, Shi Rong, Wang Tianming, Wu Jiasheng, Ma Yueming, Cheng Nengneng
Laboratory of Pharmacokinetics, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
Biomed Chromatogr. 2011 Jul;25(7):816-26. doi: 10.1002/bmc.1521. Epub 2010 Sep 27.
A sensitive and specific liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method was developed and validated to simultaneously quantify 11 active compounds (coptisine, jatrorrhizine, berberine, palmatine, baicalin, baicalein, wogonoside, wogonin, rhein, emodin and aloeemodin) from Xiexin decoction (XXD) in rat plasma. Plasma samples extracted by a single-step protein precipitation procedure were separated using the gradient mode on a Dikma ODS-C₁₈ column. Selected reaction monitoring scanning was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. Calibration curves offered satisfactory linearity (r > 0.995) at linear range of 0.47-60 ng/mL for coptisine, jatrorrhizine, berberine and palmatine, 15-1930 ng/mL for baicalin, 20-2560 ng/mL for baicalein, 14-1790 ng/mL for wogonoside, 0.57-72.8 ng/mL for wogonin, 10-1280 ng/mL for rhein, 0.6-76.8 ng/mL for emodin and 3.0-384 ng/mL for aloeemodin. The intra- and interday precisions were less than 10.2% in terms of relative standard deviation (RSD), and the accuracies were within ±10.84% in terms of relative error (RE). It was successfully applied to the evaluation of pharmacokinetics after single oral doses of XXD were administered to rats.
建立并验证了一种灵敏且特异的液相色谱 - 电喷雾电离 - 串联质谱（LC - ESI - MS/MS）方法，用于同时定量大鼠血浆中泻心汤（XXD）的11种活性成分（黄连碱、药根碱、小檗碱、巴马汀、黄芩苷、黄芩素、汉黄芩苷、汉黄芩素、大黄酸、大黄素和芦荟大黄素）。通过单步蛋白沉淀法提取的血浆样品，在迪马ODS - C₁₈柱上采用梯度模式进行分离。采用选择反应监测扫描进行定量，在一次运行中通过切换电喷雾离子源极性在正、负模式之间进行。校准曲线在0.47 - 60 ng/mL（黄连碱、药根碱、小檗碱和巴马汀）、15 - 1930 ng/mL（黄芩苷）、20 - 2560 ng/mL（黄芩素）、14 - 1790 ng/mL（汉黄芩苷）、0.57 - 72.8 ng/mL（汉黄芩素）、10 - 1280 ng/mL（大黄酸）、0.6 - 76.8 ng/mL（大黄素）和3.0 - 384 ng/mL（芦荟大黄素）的线性范围内具有良好的线性（r＞0.995）。日内和日间精密度的相对标准偏差（RSD）小于10.2%，准确度的相对误差（RE）在±10.84%以内。该方法成功应用于大鼠单次口服XXD后的药代动力学评价。
