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一种用于同时测定八种生物活性成分的简单灵敏的 HPLC 方法及五味子的指纹图谱分析。

A simple and sensitive HPLC method for the simultaneous determination of eight bioactive components and fingerprint analysis of Schisandra sphenanthera.

机构信息

Department of Pharmacy, Changzheng Hospital, Second Military Medical University, Shanghai 200003, China.

出版信息

Anal Chim Acta. 2010 Mar 3;662(1):97-104. doi: 10.1016/j.aca.2009.12.039. Epub 2010 Jan 11.

Abstract

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.

摘要

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。

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