Halstead C W, Lee S, Khoo C S, Hennell J R, Bensoussan A
Herbal Analysis Laboratory (HAL), Centre for Complementary Medicine Research, University of Western Sydney, Campbelltown, NSW, 2560, Australia.
Herbal Analysis Laboratory (HAL), Centre for Complementary Medicine Research, University of Western Sydney, Campbelltown, NSW, 2560, Australia.
J Pharm Biomed Anal. 2007 Sep 21;45(1):30-37. doi: 10.1016/j.jpba.2007.05.016. Epub 2007 May 21.
A rapid and specific reversed-phase high performance liquid chromatography (RP-LC) method with photodiode array detection (DAD) was developed and validated for the determination of four common schisandra lignans, schisandrin (1), schisandrol B (2), deoxyshisandrin (3) and gamma-schisandrin (4), in raw herb materials and commercial dried aqueous extracts of Schisandra chinensis (Wu Wei Zi). The extraction solvent and extraction method were optimised where it was found that a 4 h Soxhlet extraction using methanol was successful at extracting >99.5% of each of the schisandra lignans analysed from the raw herb material. The sample preparation process for the dried aqueous extract samples involved sonication using methanol for 2 x 30 min. The herb and extract solutions were separated on a Varian Microsorb-MV 100-5 C18 column using a gradient mixture of 0.1% aqueous phosphoric acid and acetonitrile. Subsequent detection and quantitation of the schisandra lignans was performed at 210 nm. The correlation coefficients of the linear regression analysis performed on these calibration curves were >0.9996 for all four schisandra lignans assayed. The detection limits and quantification limits ranged from 0.12 to 0.57 and 0.41 to 1.89 mg g(-1), respectively. The mean recoveries of the various analytes ranged from 92.20 to 107.01%. The method was used to investigate the levels of the four mentioned components in herb samples and dried aqueous extracts. The identities of the chromatographic peaks were confirmed by (+) electrospray ionisation LC-MS/MS.
建立了一种快速、特异的反相高效液相色谱(RP-LC)法,并采用光电二极管阵列检测(DAD),用于测定五味子(Wu Wei Zi)生药材和市售干燥水提取物中四种常见的五味子木脂素,即五味子醇甲(1)、五味子醇乙(2)、脱氧五味子醇甲(3)和γ-五味子醇甲(4)。对提取溶剂和提取方法进行了优化,发现用甲醇进行4小时索氏提取能够成功提取生药材中分析的每种五味子木脂素的>99.5%。干燥水提取物样品的样品制备过程包括用甲醇超声处理2×30分钟。药材和提取物溶液在Varian Microsorb-MV 100-5 C18柱上分离,使用0.1%磷酸水溶液和乙腈的梯度混合物。随后在210nm处对五味子木脂素进行检测和定量。对这些校准曲线进行线性回归分析得到的相关系数,对于所有四种测定的五味子木脂素均>0.9996。检测限和定量限分别为0.12至0.57和0.41至1.89mg g(-1)。各种分析物的平均回收率为92.20至107.01%。该方法用于研究药材样品和干燥水提取物中上述四种成分的含量。通过(+)电喷雾电离LC-MS/MS确认了色谱峰的身份。