Department of Pharmacy, Changzheng Hospital, Second Military Medical University, Shanghai 200003, China.
Anal Chim Acta. 2010 Mar 3;662(1):97-104. doi: 10.1016/j.aca.2009.12.039. Epub 2010 Jan 11.
A simple and sensitive high performance liquid chromatography method with photodiode array detection (HPLC-DAD) was developed for simultaneous determination of eight bioactive constituents (schisandrin, schisandrol B, schisantherin A, schisanhenol, anwulignan, deoxyshisandrin, schisandrin B and schisandrin C) in the ripe fruit of Schisandra sphenanthera and its traditional Chinese herbal preparations Wuzhi-capsule by optimizing the extraction, separation and analytical conditions of HPLC-DAD. The chemical fingerprint of S. sphenanthera was established using raw materials of 15 different origins in China. The chromatographic separations were obtained by an Agilent Eclipse XDB-C18 reserved-phase column (250 mm x 4.6 mm i.d., 5 microm) using gradient elution with water-formic acid (100:0.1, v/v) and acetonitrile, at a flow rate of 1.0 mL min(-1), an operating temperature of 35 degrees C, and a wavelength of 230 nm. The constituents were confirmed by (+) electrospray ionization LC-MS. The new method was validated and was successfully applied to simultaneous determination of components in 13 batches of Wuzhi-capsule. The results indicate that this multi-component determination method in combination with chromatographic fingerprint analysis is suitable for quantitative analysis and quality control of S. sphenanthera.
建立了一种简单、灵敏的高效液相色谱-二极管阵列检测(HPLC-DAD)法,用于同时测定五味子成熟果实及其中药制剂五酯胶囊中 8 种生物活性成分(五味子甲素、五味子醇 B、五味子酯甲、五味子酚、戈米辛 L、去氧五味子素、五味子乙素和五味子丙素)。通过优化 HPLC-DAD 的提取、分离和分析条件,对其进行了优化。采用中国 15 个不同产地的五味子原料,建立了五味子的化学指纹图谱。采用 Agilent Eclipse XDB-C18 保留相柱(250mm×4.6mm id,5μm),以水-甲酸(100:0.1,v/v)和乙腈为流动相,梯度洗脱,流速为 1.0ml/min,柱温为 35℃,检测波长为 230nm,实现了色谱分离。采用(+)电喷雾电离 LC-MS 对各成分进行确认。对新方法进行了验证,并成功应用于 13 批五酯胶囊中成分的同时测定。结果表明,该多组分测定方法结合色谱指纹图谱分析,适用于五味子的定量分析和质量控制。