Zhang Xiaowen, Li Qing, Lv Chunxiao, Xu Huarong, Liu Xujia, Sui Zhenyu, Bi Kaishun
School of Chinese Material Medica, Shenyang Pharmaceutical University, Shenyang, China.
National and Local United Engineering Laboratory for Key Technology of Chinese Material Medica Quality Control, Shenyang Pharmaceutical University, Shenyang, China.
J Sep Sci. 2015 Jun;38(12):2068-75. doi: 10.1002/jssc.201500123. Epub 2015 May 7.
A sensitive and reliable ultra high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry method was established to separate and identify the chemical constituents of Kai-Xin-San prescription, a classic traditional Chinese medicine formula that plays an important role in the treatment of Alzheimer's disease. The detection was performed on an Agilent 6520 Accurate-Mass quadrupole time-of-flight mass spectrometer equipped with an electrospray ionization source in negative modes. With the optimized conditions, a total of 54 compounds were identified or tentatively characterized. Out of the 54 compounds, six compounds were identified by comparing the retention time and mass spectrometry data with reference standards, the rest were characterized by analyzing mass spectrometry data and retrieving the literature data. Results indicated ginsenosides, polygala saponins, terpenoids, and oligosaccharide esters were the major effective constituents in Kai-Xin-San prescription. There were 26 prototype ingredients that were assigned for identification in rat plasma. It is also concluded that the developed ultra high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry method with high sensitivity and resolution is suitable for identifying and characterizing the chemical constituents of Kai-Xin-San prescription, and the analysis provides a helpful chemical basis for further research on Kai-Xin-San prescription and the clinical diagnostics of Alzheimer's disease.
建立了一种灵敏可靠的超高效液相色谱-四极杆-飞行时间质谱联用方法，用于分离和鉴定开心散方剂中的化学成分。开心散是一种经典的中药方剂，在治疗阿尔茨海默病中发挥着重要作用。检测在配备电喷雾电离源的安捷伦6520精确质量四极杆飞行时间质谱仪上以负离子模式进行。在优化条件下，共鉴定或初步表征了54种化合物。在这54种化合物中，通过将保留时间和质谱数据与参考标准品进行比较，鉴定出6种化合物，其余化合物通过分析质谱数据并检索文献数据进行表征。结果表明，人参皂苷、远志皂苷、萜类化合物和低聚糖酯是开心散方剂中的主要有效成分。在大鼠血浆中鉴定出26种原型成分。还得出结论，所建立的具有高灵敏度和分辨率的超高效液相色谱-四极杆-飞行时间质谱联用方法适用于鉴定和表征开心散方剂中的化学成分，该分析为开心散方剂的进一步研究和阿尔茨海默病的临床诊断提供了有益的化学依据。
