Cheng Xing-Ye, Shi Yue, Zhen Shun-Liang, Sun Hong, Jin Wen
Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100094, China.
J Chromatogr Sci. 2010 Jul;48(6):441-4. doi: 10.1093/chromsci/48.6.441.
An accurate and simple analysis method by high-performance liquid chromatography (HPLC)-electrospray tandem mass spectrometry (ESI-MS-MS) for the ethanol extract of Corydalis yanhusuo was established in this study. In this method, a C(18) column was used, and the mobile phase was water (0.2% acetic acid, 0.1% triethylamine, v/v)-acetonitrile (24:76, v/v). Under the optimal analysis conditions established in this study, eight protoberberine quaternary alkaloids in the ethanol extract of Corydalis yanhusuo were well separated and identified, respectively. Eight regression equations showed a good linear relationship between the peak area of each marker and concentration (r = 0.9990-0.9995). The various other aspects of analysis (i.e., peak purity, precision, recovery, and repeatability) were also validated. For the eight components, the recoveries were found to be 98.9%, 99.2%, 105.0%, 97.7%, 101.4%, 98.6%, 98.5%, and 98.7%, respectively. The limits of detection were 14.6, 42.5, 22.4, 17.9, 25.4, 10.0, 18.7, 3.9 ng/mL, respectively, and the limits of quantitation were 48.6, 141.7, 74.6, 59.6, 84.8, 33.2, 62.3, and 12.9 ng/mL, respectively. The developed method is useful for the simultaneous determination of these alkaloids in a large number of ethanol extracts of Corydalis yanhusuo.
本研究建立了一种采用高效液相色谱（HPLC）-电喷雾串联质谱（ESI-MS-MS）准确、简便分析延胡索乙醇提取物的方法。该方法采用C(18)柱，流动相为水（0.2%乙酸、0.1%三乙胺，v/v）-乙腈（24:76，v/v）。在本研究建立的最佳分析条件下，延胡索乙醇提取物中的8种原小檗碱季铵生物碱得到了良好的分离和鉴定。8个回归方程表明各标志物的峰面积与浓度之间具有良好的线性关系（r = 0.9990 - 0.9995）。分析的其他各个方面（即峰纯度、精密度、回收率和重复性）也得到了验证。对于这8种成分，回收率分别为98.9%、99.2%、105.0%、97.7%、101.4%、98.6%、98.5%和98.7%。检测限分别为14.6、42.5、22.4、17.9、25.4、10.0、18.7、3.9 ng/mL，定量限分别为48.6、141.7、74.6、59.6、84.8、33.2、62.3和12.9 ng/mL。所建立的方法可用于同时测定大量延胡索乙醇提取物中的这些生物碱。
