电堆积大体积进样-在线扫集-胶束毛细管电动色谱法测定胡黄连中的4种有机酸

Separation and Determination of Four Organic Acids in Picrorhiza Scrophulariiflora Pennell by Electrostacking-Large Volume Sample Stacking-Sweeping-Micellar Electrokinetic Chromatography

建立了以电堆积大体积进样-在线扫集-胶束毛细管电动色谱法测定胡黄连中的异阿魏酸、肉桂酸、阿魏酸和香草酸的新方法。考察了pH值、四硼酸钠浓度、SDS浓度、电压、有机溶剂和进样时间对分离效果的影响。以40 mmol/L四硼酸钠-80 mmol/L十二烷基磺酸钠(SDS)为缓冲液(含10%(V/V)甲醇,pH 9.4),在进样电压-10 kV,分离电压20 kV,检测波长214 nm,环境温度25℃的条件下,达到最佳的分离效果。异阿魏酸、肉桂酸、阿魏酸和香草酸的线性范围分别为16～543μg/L,16～518μg/L,18～589μg/L和14～161μg/L;回收率分别为93%～111%,102%～107%,96%～108%和103%～108%;峰面积的RSD均小于4%;4种有机酸的检出限分别为618,148,368和76 ng/L。

A novel method for simultaneous determination of four organic acids,isoferulic acid,cinnamic acid,ferulic acid and vanillic acid,in picrorhiza scrophulariiflora pennell by electrostacking-large volume sample stacking-sweeping micellar electrokinetic chromatography has been proposed.The determination conditions containing pH in background solution,concentration of Na2B4O7,sodium dodecyl sulfate（SDS） and methanol,injection time,injection voltage,separation voltage were optimized.The operating buffer was composed of 40 mmol/L Na2B4O7,80 mmol/L SDS and 10%（by volume） methanol at pH 9.4 with a constant temperature of 25 ℃.The UV detection wavelength was 214 nm,the applied voltage was-10 kV,separation voltage was 20 kV and injection time was 450 s.The linear ranges of the method were 16-543 μg/L for Isforerulic acid,16-518 μg/L for Cinnamic acid,18-589 μg/L for Ferulic acid and 14-161 μg/L for Vanillic acid.The recoveries were 93%-111%,102%-107%,96%-108%,103%-108%,respectively.And the RSDs of peak area were less than 4%,and detection limits（S/N=3） were 618,148,368 and 76 ng/L for four organic acids respectively.