College of Pharmacy, Qiqihar Medical University, Qiqihar 161006, Heilongjiang, China.
Molecules. 2017 Sep 11;22(9):1524. doi: 10.3390/molecules22091524.
A method based on a simplified extraction by matrix solid phase dispersion (MSPD) followed by ultra-performance liquid chromatography coupled with the quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS) determination is validated for analysis of two phenolics and three terpenoids in . The optimized experimental parameters of MSPD including dispersing sorbent (silica gel), ratio of sample to dispersing sorbent (1:2), elution solvent (water-ethanol: 30-70) and volume of the elution solvent (10 mL) were examined and set down. The highest extraction yields of chromatogram information and the five compounds were obtained under the optimized conditions. A total of 25 constituents have been identified and five components have been quantified from . A linear relationship (r² ≥ 0.9964) between the concentrations and the peak areas of the mixed standard substances were revealed. The average recovery was between 92.4% and 103.2% with RSD values less than 3.45% ( = 5). The extraction yields of two phenolics and three terpenoids obtained by the MSPD were higher than those of traditional reflux and sonication extraction with reduced requirement on sample, solvent and time. In addition, the optimized method will be applied for analyzing terpenoids in other Chinese herbal medicine samples.
基于简化的基质固相分散（MSPD）提取，结合超高效液相色谱与四极杆飞行时间串联质谱（UPLC/Q-TOF-MS）检测法，验证了 中两种酚类和三种萜类化合物的分析方法。对 MSPD 的实验参数（硅胶作为分散吸附剂、样品与分散吸附剂的比例 1:2、洗脱溶剂（水-乙醇：30-70）和洗脱溶剂的体积（10mL））进行了优化，并确定下来。在优化条件下，可获得色谱信息和五种化合物的最高提取产率。从 中共鉴定出 25 种成分，并对其中 5 种成分进行了定量分析。混合标准物质的浓度与峰面积之间存在良好的线性关系（r²≥0.9964）。平均回收率在 92.4%至 103.2%之间，RSD 值小于 3.45%（n=5）。与传统回流和超声提取相比，MSPD 法提取两种酚类和三种萜类化合物时，所需样品、溶剂和时间更少，提取产率更高。此外，该优化方法将应用于分析其他中草药样品中的萜类化合物。
