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目的 :以超临界流体萃取 ( SFE)银杏叶粗提物中槲皮素和山奈素 ,以胶束电动毛细管色谱法 ( MECC)测定这两种成分的含量。 方法 :采用正交设计法考察 SFE提取工艺 ,SFE条件 :压力 42 m Pa;温度 6 0℃ ;静态萃取时间 4m in;动态萃取体积 4m l;改性剂 0 .2 ml乙醇。 MECC条件 :空心熔融石英毛细管柱 ( 5 5 cm× 75μm ) ;缓冲液为磷酸二氢钠 -硼砂 =2 5 - 6 .2 5mm ol/L ( p H 8.5 ) ;SDS 35 mmol/L ;检测波长 2 5 4nm。结果 :SFE时改性剂对萃取效率的影响最大 ;MECC以肉桂酸为内标 ,在 2 1.2～ 10 6 .0μg/ml和 2 0 .0～ 10 0 .0μg/ml范围内 ,槲皮素和山奈素均呈良好的线性关系和重现性。 40 ,6 0和 80μl槲皮素的加样回收率分别为 93.87% ,94.0 2 %和 94.10 % ;40 ,6 0和 80μl山奈素的加样回收率分别为 94.5 0 % ,94.17%和 94.2 5 %。结论 :SFE与 MECC法联用 ,简便快速 ,可用于银杏叶粗提物中的黄酮类成分的分离分析。
PURPOSE: To determine the contents of these two components by means of micellar electrokinetic capillary chromatography (MECC) with supercritical fluid extraction (SFE) of quercetin and kaempferol in crude Ginkgo biloba extracts. Methods: The orthogonal design method was used to investigate the SFE extraction process. SFE conditions: pressure 42 m Pa; temperature 60 °C; static extraction time 4 m in; dynamic extraction volume 4 m l; modifier 0.2 ml ethanol. MECC conditions: Hollow fused silica capillary column (55 cm×75 μm); Buffer sodium dihydrogen phosphate-borax=25-6.25 mmol/L (p H 8.5 ); SDS 35 mmol/L; detection wavelength 2 5 4nm. Results: The effect of the modifier on the extraction efficiency was greatest at SFE; MECC with cinnamic acid as the internal standard, in the range of 2 1.2 to 10 6 .0 μg/ml and 2 0 . to 10 0 .0 μg/ml, quercetin Both of them show good linearity and reproducibility with kaempferol. The recoveries of 40, 60, and 80 μl of quercetin were 93.87%, 94.0 2%, and 94.10 %, respectively. The recoveries of 40, 60, and 80 μl of kaempferol were 94.5 0 %, 94.17%, and 94.2 5 respectively. %. Conclusion : The combination of SFE and MECC is simple and rapid. It can be used for the separation and analysis of flavonoids in Ginkgo biloba extract.