Wang Zhibing, Ma Siyu, Zhang Qian, He Shuang, Li Qing, Hu Jianxue, Zhang Hanqi
College of Chemistry and Life Science, Changchun University of Technology, Changchun, 130012, P.R. China.
College of Chemistry, Jilin University, Changchun 130012, P.R. China.
J Chromatogr Sci. 2017 Mar 1;55(3):316-326. doi: 10.1093/chromsci/bmw187.
A simple, rapid and efficient method based on matrix solid-phase dispersion coupled with high-performance liquid chromatography was developed for determination of lipophilic constituents, including dihydrotanshinone, tanshinone I, cryptotanshinone and tanshinone II A in Salvia miltiorrhiza Bunge Box-Behnken design was employed for optimization of the extraction conditions of matrix solid-phase dispersion, including mass ratio of dispersant to sample, volume of elution solvent, and amount of cleanup reagent. The optimal experimental results were obtained using 0.27 g of acid alumina as dispersant, 13 mL of acetonitrile as elution solvent and 0.36 g of acid alumina as cleanup reagent. The target analytes was determined by high-performance liquid chromatography. The recoveries of tanshinones obtained by analyzing the spiked samples were from 83.81% to 93.74% and relative standard deviations from 2.87% to 6.83%. Matrix solid-phase dispersion integrated the extraction and cleanup into a single step, which provides the advantages of being simple, fast and convenient. Compared with other conventional methods, the present method consumed less time and less organic solvent. The results demonstrate that this method has potential for the determination of active constituents and the quality control of traditional Chinese medicine.
建立了一种基于基质固相分散结合高效液相色谱法的简单、快速、高效的方法，用于测定丹参中的亲脂性成分，包括二氢丹参酮、丹参酮I、隐丹参酮和丹参酮IIA。采用Box-Behnken设计优化基质固相分散的提取条件，包括分散剂与样品的质量比、洗脱溶剂体积和净化试剂用量。以0.27 g酸性氧化铝为分散剂、13 mL乙腈为洗脱溶剂、0.36 g酸性氧化铝为净化试剂时，获得了最佳实验结果。采用高效液相色谱法测定目标分析物。加标样品分析得到的丹参酮回收率为83.81%至93.74%，相对标准偏差为2.87%至6.83%。基质固相分散将提取和净化整合为一步，具有简单、快速、方便的优点。与其他传统方法相比，本方法耗时更少，有机溶剂消耗更少。结果表明，该方法在中药活性成分测定和质量控制方面具有应用潜力。
