College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, China.
State Key Laboratory Cultivation Base for TCM Quality and Efficacy, Nanjing University of Chinese Medicine, Nanjing, China.
J Sep Sci. 2018 Jun;41(11):2310-2320. doi: 10.1002/jssc.201701408. Epub 2018 Mar 15.
We established a rapid and sensitive ultra high-performance liquid chromatography tandem mass spectrometry method for the simultaneous quantification of xanthones and steroidal saponins in rat plasma. Chromatographic separation was achieved on a C column with a mobile phase comprising acetonitrile and 0.1% formic acid. The detection was performed by negative electrospray ionization in multiple reaction monitoring mode. The validated method showed good linearity within the tested range (r > 0.9945). The intra- and interday precision at high, medium, and low concentrations was less than 7.96%. The bias of accuracies ranged from -1.92 to 9.62%. The extraction recoveries of the compounds ranged from 84.78 to 88.69%, and the matrix effects ranged from 96.76 to 108.59%. This method was successfully applied to a pharmacokinetic comparison of crude and salt-processed Anemarrhenae Rhizoma aqueous extracts after oral administration in rats. The maximum plasma concentration and area under concentration-time curve of timosaponin BIII and timosaponin AIII increased significantly (P < 0.05 or 0.01) and those of timosaponin BII decreased significantly (P < 0.05) after processing. These results could contribute to the clinical application of crude and salt-processed Anemarrhenae Rhizoma and reveal the processing mechanism.
我们建立了一种快速灵敏的超高效液相色谱串联质谱法，用于同时定量大鼠血浆中的姜黄素和甾体皂苷。色谱分离在 C 柱上进行，流动相由乙腈和 0.1%甲酸组成。检测采用负离子电喷雾电离多反应监测模式进行。验证后的方法在测试范围内具有良好的线性（r>0.9945）。高、中、低浓度下的日内和日间精密度均小于 7.96%。准确度的偏差范围为-1.92 至 9.62%。化合物的提取回收率在 84.78%至 88.69%之间，基质效应在 96.76%至 108.59%之间。该方法成功应用于大鼠口服生地黄和盐地黄水提物的药代动力学比较。处理后，知母皂苷 BIII 和知母皂苷 AIII 的最大血浆浓度和浓度-时间曲线下面积显著增加（P<0.05 或 0.01），知母皂苷 BII 的浓度显著降低（P<0.05）。这些结果有助于生地黄和盐地黄的临床应用，并揭示了炮制机制。
