Jiang Y, Li S P, Chang H T, Wang Y T, Tu P F
School of Pharmaceutical Sciences, Health Science Center of Peking University, Beijing, China.
J Chromatogr A. 2006 Mar 10;1108(2):268-72. doi: 10.1016/j.chroma.2006.01.077. Epub 2006 Feb 3.
A new method based on pressurized liquid extraction (PLE) followed by a sensitive and specific HPLC-DAD analysis is developed for determination of seven compounds in Cortex Dictamni. The operational parameters of PLE, such as extraction solvent, extraction temperature, extraction pressure, static extraction time, flush volume and extraction cycles were optimized, using the extraction efficiencies of dictamnine, obacunone and fraxinellone as targets. The optimized procedure employed MeOH as extraction solvent, 150 degrees C of extraction temperature, 1,500 psi extraction pressure, 5 min of static extraction time, 60% flush volume and the extraction recoveries of the three compounds were nearly to 100% for only one cycle. The following HPLC analysis was performed on a reversed-phase C(18) column with methanol-water as mobile phase in gradient manner, detected at 236 and 218 nm. The limits of detection (LOD) and limits of quantification (LOQ) of the seven compounds were in the range of 0.4-15.6 ng and 1.2-38.8 ng. This assay can be readily utilized as a quality control method for Cortex Dictamni and other related medicinal plants.
建立了一种基于加压液体萃取(PLE)并结合灵敏且特异的高效液相色谱-二极管阵列检测(HPLC-DAD)分析方法,用于测定白鲜皮中的七种化合物。以白鲜碱、黄柏酮和吴茱萸次碱的提取效率为指标,对PLE的操作参数,如提取溶剂、提取温度、提取压力、静态提取时间、冲洗体积和提取次数进行了优化。优化后的方法采用甲醇作为提取溶剂,提取温度为150℃,提取压力为1500 psi,静态提取时间为5分钟,冲洗体积为60%,仅一个提取循环,三种化合物的提取回收率就接近100%。随后的HPLC分析在反相C18柱上进行,以甲醇-水为流动相进行梯度洗脱,在236 nm和218 nm处检测。七种化合物的检测限(LOD)和定量限(LOQ)在0.4 - 15.6 ng和1.2 - 38.8 ng范围内。该方法可作为白鲜皮及其他相关药用植物的质量控制方法。