School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, P. R. China.
Jiangsu Key Laboratory of Chinese Medicine Processing, Nanjing University of Chinese Medicine, Nanjing, P. R. China.
J Sep Sci. 2017 Apr;40(8):1686-1693. doi: 10.1002/jssc.201601459. Epub 2017 Mar 21.
A rapid and sensitive ultra-high performance liquid chromatography with tandem mass spectrometry approach was established for the simultaneous determination of 4-caffeoylquinic acid, loganic acid, chlorogenic acid, loganin, 3,5-dicaffeoylquinic acid, dipsacoside B, asperosaponin VI, and sweroside in raw and wine-processed Dipsacus asper. Chloramphenicol and glycyrrhetinic acid were employed as internal standards. The proposed approach was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery. Intra- and interassay variability for all analytes were 2.8-4.9 and 1.7-4.8%, respectively. The standard addition method determined recovery rates for each analytes (96.8-104.6%). In addition, the developed approach was applied to 20 batches of raw and wine-processed samples of Dipsacus asper. Principle component analysis and partial least squares-discriminate analysis revealed a clear separation between the raw group and wine-processed group. After wine-processing, the contents of loganic acid, chlorogenic acid, dipsacoside B, and asperosaponin VI were upregulated, while the contents of 3,5-dicaffeoylquinic acid, 4-caffeoylquinic acid, loganin, and sweroside were downregulated. Our results demonstrated that ultra-high performance liquid chromatography with tandem mass spectrometry quantification combined with chemometrics is a viable method for quality evaluation of the raw Dipsacus asper and its wine-processed products.
建立了一种快速灵敏的超高效液相色谱-串联质谱法,用于同时测定生地黄和酒地黄中 4-咖啡酰奎宁酸、龙胆酸、绿原酸、马钱苷、3,5-二咖啡酰奎宁酸、毛蕊花糖苷 B、柴胡皂苷 VI 和梓醇的含量。氯霉素和甘草酸被用作内标。该方法在线性、灵敏度、精密度、重复性和回收率方面均得到了全面验证。所有分析物的日内和日间变异性分别为 2.8-4.9%和 1.7-4.8%。标准加入法确定了每个分析物的回收率(96.8-104.6%)。此外,该方法还应用于 20 批生地黄和酒地黄的样品。主成分分析和偏最小二乘判别分析显示,生地黄组和酒地黄组之间有明显的分离。酒制后,龙胆酸、绿原酸、毛蕊花糖苷 B 和柴胡皂苷 VI 的含量升高,而 3,5-二咖啡酰奎宁酸、4-咖啡酰奎宁酸、马钱苷和梓醇的含量降低。研究结果表明,超高效液相色谱-串联质谱联用结合化学计量学是评价生地黄及其酒制品质量的一种可行方法。