Wang Ying, Zhang Yifan, Xiao Juan, Xu Ranchi, Wang Qiangli, Wang Xinhong
School of Pharmacy, Shanghai University of Traditional Chinese Medicine, Shanghai, China.
School of Pharmacy, Shanghai University of Medicine and Health Sciences, Shanghai, China.
Biomed Chromatogr. 2018 Feb;32(2). doi: 10.1002/bmc.4083. Epub 2017 Oct 2.
A rapid and high-sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for simultaneous determination of nine active constituents (baicalin, baicalein, wogonoside, wogonin, scutellarin, berberine, coptisine, ginsenoside Rb1 and ginsenoside Re) in rat plasma after oral administration of Banxia xiexin decoction (BXD). Biological samples were processed wtih acetone-ethyl acetate (4:1, v/v). The mobile phase consisted of methanol and water (containing 0.1% formic acid) with gradient elution at a flow rate of 0.3 mL/min. Detection was performed on a triple quadrupole mass spectrometer using positive ion and negative ESI in the multiple reaction monitoring mode. The calibration curves for all analytes had good linearity (r > 0.9933). The mean recovery of all the nine active ingredients was >75.2%, and the intra- and inter-day precisions were within 12.0%; the accuracy was between 87.4 and 110.4%. This method was successfully applied to a pharmacokinetic study after administration of BXD. The results of the pharmacokinetic study might be helpful for BXD reasonable clinical application and further studies on mechanism.
建立了一种快速、高灵敏度的液相色谱/串联质谱(LC/MS/MS)方法,用于同时测定大鼠口服半夏泻心汤(BXD)后血浆中的9种活性成分(黄芩苷、黄芩素、汉黄芩苷、汉黄芩素、野黄芩苷、小檗碱、黄连碱、人参皂苷Rb1和人参皂苷Re)。生物样品用丙酮-乙酸乙酯(4:1,v/v)处理。流动相由甲醇和水(含0.1%甲酸)组成,采用梯度洗脱,流速为0.3 mL/min。在三重四极杆质谱仪上采用正离子和负电喷雾电离(ESI),在多反应监测模式下进行检测。所有分析物的校准曲线均具有良好的线性(r>0.9933)。9种活性成分的平均回收率均>75.2%,日内和日间精密度均在12.0%以内;准确度在87.4%至110.4%之间。该方法成功应用于BXD给药后的药代动力学研究。药代动力学研究结果可能有助于BXD的合理临床应用及作用机制的进一步研究。