Ma Sai, Chen Lingxin, Luo Guoan, Ren Kangning, Wu Juanfang, Wang Yiming
Department of Chemistry, Tsinghua University, Analysis Center, Tsinghua, Haidian, Beijing 100084, China.
J Chromatogr A. 2006 Sep 15;1127(1-2):207-13. doi: 10.1016/j.chroma.2006.06.021. Epub 2006 Jul 3.
A comprehensive two-dimensional liquid chromatography system was constructed on the combination of size exclusion chromatography (SEC) and reverse phase liquid chromatography (RPLC). The first dimension used a SEC column with 300 mm x 8mm i.d., packed with Toyopearl HW-40S. The column was eluted with 0.05 mol/l Tris-HCl (pH 6.9) at a flow rate of 0.4 ml/min. The second dimension used a RPLC column with 100 mm x 4.6mm i.d., which was operated in gradient form at a flow rate of 1.0 ml/min. An automatic switching valve was used to collect the effluent of the SEC column every 3 min, and the effluent was automatically injected into the RPLC column. Mass spectrometer was used for peak identification. This system was used to separate Qingkailing injection, a traditional Chinese medicine (TCM). The result showed that the total peak capacity of this system could reach 1134 and the qualitative analysis of seven chemical components of the Qingkailing injection was accomplished by this system. The results show that comprehensive two-dimensional liquid chromatography system is of great importance and high value in the separation of complex TCM.
构建了一种基于尺寸排阻色谱（SEC）和反相液相色谱（RPLC）联用的全二维液相色谱系统。第一维使用内径为8mm、柱长300mm、填充有Toyopearl HW - 40S的SEC柱，以0.05mol/L Tris - HCl（pH 6.9）为洗脱剂，流速为0.4ml/min进行洗脱。第二维使用内径为4.6mm、柱长100mm的RPLC柱，以1.0ml/min的流速进行梯度洗脱。使用自动切换阀每隔3分钟收集SEC柱的流出物，并将流出物自动注入RPLC柱。采用质谱仪进行峰鉴定。该系统用于分离中药清开灵注射液。结果表明，该系统的总峰容量可达1134，并完成了清开灵注射液七种化学成分的定性分析。结果表明，全二维液相色谱系统在复杂中药的分离中具有重要意义和很高的价值。
