Pharmaceutical College, Heilongjiang University of Chinese Medicine, Harbin, PR China.
J Sep Sci. 2009 Dec;32(23-24):4113-25. doi: 10.1002/jssc.200900488.
A simple and reproducible HPLC-photodiode array detector method has been described for evaluating and controlling quality of Forsythia suspensa extract (FSE). First, by analysis of chromatographic fingerprints, the similarities of chromatograms of FSE samples from the same pharmaceutical company exceeded 0.999, 0.997 and 0.960, respectively, although they were much lower from different pharmaceutical companies. Second, by further comparing many batches of extract chromatograph charts with the corresponding reference herb materials, the "common peaks" 3, 5, 7 and 10 were defined as "marker peaks", which were identified as (+)-pinoresinol-beta-D-glucoside, forsythiaside, phillyrin and phillygenin, respectively. Third, four "marker peaks" were simultaneously determined based on fingerprint chromatogram for further controlling the quality of FSE quantitatively. Namely, the newly developed method was successfully applied to analyze 38 batches of FSE samples supplied by three pharmaceutical factories, which showed acceptable linearity, intra-day precision (RSD<2.76%), inter-day precision (RSD<3.43%) and the average recovery rates in the range of (95.38+/-2.96)% to (101.60+/-3.08)%. At last, hierarchical clustering analysis and Bayes discriminant analysis statistical methods were used to classify and differentiate the 38 FSE samples to provide the basis for guiding reasonable use of FSE and controlling its quality better.
已描述了一种简单且可重现的 HPLC-光电二极管阵列检测器方法,用于评估和控制连翘提取物(FSE)的质量。首先,通过分析色谱指纹图谱,来自同一制药公司的 FSE 样品的图谱相似度分别超过了 0.999、0.997 和 0.960,尽管它们来自不同的制药公司时则低得多。其次,通过进一步比较许多批提取物的色谱图与相应的参考草药材料,将“共同峰”3、5、7 和 10 定义为“标记峰”,分别鉴定为(+)-松脂醇-β-D-葡萄糖苷、连翘苷、连翘酯苷和连翘苷元。第三,基于指纹图谱同时测定了四个“标记峰”,以进一步定量控制 FSE 的质量。即,成功地将新开发的方法应用于分析三个制药厂提供的 38 批 FSE 样品,结果表明该方法具有良好的线性、日内精密度(RSD<2.76%)、日间精密度(RSD<3.43%)和平均回收率在(95.38+/-2.96)%至(101.60+/-3.08)%范围内。最后,使用层次聚类分析和贝叶斯判别分析统计方法对 38 批 FSE 样品进行分类和区分,为指导 FSE 的合理使用和更好地控制其质量提供了依据。