Yang Xiaorong, Xiang Qingxiang, Chen Jiaxuan
Department of Chemistry and Life Science, Leshan Teachers College, Leshan 614004, China.
Se Pu. 2009 May;27(3):313-7.
The systems of mobile phase for the determination of gamma-schisandrin in Schisandra chinensis and its preparations were developed by high performance liquid chromatography (HPLC). The separation was performed on a Shim-pack VP-ODS column (250 mm x 4.6 mm, 5 microm) at 30 degrees C, the detection wavelength was set at 285 nm and the flow rate was 1.0 mL/min. Retention times and separation were investigated in mixed solution of three reference substances (gamma-schisandrin, anwulignan, and deoxyschizandrin) and methanol extract of Schisandra chinensis by different systems and proportions of mobile phases to select optimal conditions for the determination of gamma-schisandrin. The results showed that the complete separation of gamma-schisandrin and anwulignan was difficult in the systems of methanol-water and methanol-acetic acid-water. The separation of gamma-schisandrin, anwulignan and deoxyschizandrin can be completed in the systems of acetonitrile-methanol-water and acetonitrile-acetic acid-water when their proportions were suitable. The mobile phase of acetonitrile-methanol-water (17:58:25, v/v/v) was selected for the determination of deoxyschizandrin, gamma-schisandrin and anwulignan in Schisandra chinensis and Hugan tablets. The determination results of the three substances were satisfactory with the relative standard deviations (n = 4) ranged from 0.95% to 5.8%, and the average recoveries ranged from 94.50% to 105.6%. The efficiency of separation and the results of determination were satisfactory for the real samples.
采用高效液相色谱法(HPLC)建立了五味子及其制剂中γ-五味子醇甲含量测定的流动相系统。分离在Shim-pack VP-ODS柱(250 mm×4.6 mm,5μm)上于30℃进行,检测波长设定为285 nm,流速为1.0 mL/min。通过不同的流动相系统和比例,研究了三种对照品(γ-五味子醇甲、安五脂素和五味子甲素)混合溶液以及五味子甲醇提取物中各成分的保留时间和分离情况,以选择测定γ-五味子醇甲的最佳条件。结果表明,在甲醇-水和甲醇-乙酸-水系统中,γ-五味子醇甲和安五脂素难以完全分离。当乙腈-甲醇-水和乙腈-乙酸-水系统的比例适当时,γ-五味子醇甲、安五脂素和五味子甲素能够完全分离。选择乙腈-甲醇-水(17:58:25,v/v/v)作为流动相,用于测定五味子和护肝片中五味子甲素、γ-五味子醇甲和安五脂素的含量。三种成分的测定结果令人满意,相对标准偏差(n = 4)为0.95%至5.8%,平均回收率为94.50%至105.6%。实际样品的分离效率和测定结果均令人满意。