Wu Hongliang, Li Guoliang, Liu Shucheng, Liu Di, Chen Guang, Hu Na, Suo Yourui, You Jinmao
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining, People's Republic of China; College of Life Sciences, University of Chinese Academy of Sciences, Beijing, People's Republic of China.
Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu, People's Republic of China.
J Pharm Biomed Anal. 2015 Mar 25;107:98-107. doi: 10.1016/j.jpba.2014.10.031. Epub 2014 Nov 7.
A novel analytical method was developed for simultaneous determination of six triterpenic acids using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) follow by high-performance liquid chromatography (HPLC) with fluorescence detection. Six triterpenic acids (ursolic acid, oleanolic acid, betulinic acid, maslinic acid, betulonic acid and corosolic acid) were extracted by UA-DLLME using chloroform and acetone as the extraction and disperser solvents, respectively. After the extraction and nitrogen flushing, the extracts were rapidly derivatized with 2-(12,13-dihydro-7H-dibenzo[a,g]carbazol-7-yl)ethyl4-methylbenzenesulfonate. The main experimental parameters affecting extraction efficiency and derivatization yield were investigated and optimized by response surface methodology (RSM) combined with Box-Behnken design (BBD). The limits of detection (LODs) and the limits of quantification (LOQs) were in the range of 0.95-1.36 ng mL(-1) and 3.17-4.55 ng mL(-1), respectively. Under the optimum conditions, the method has been successfully applied for the analysis of triterpenic acids in six different traditional Chinese medicinal herbs.
建立了一种新型分析方法，采用超声辅助分散液液微萃取（UA-DLLME）结合高效液相色谱（HPLC）荧光检测法同时测定六种三萜酸。分别以氯仿和丙酮作为萃取溶剂和分散剂，通过UA-DLLME萃取六种三萜酸（熊果酸、齐墩果酸、桦木酸、山楂酸、桦酮酸和科罗索酸）。萃取并经氮气吹扫后，萃取物用2-(12,13-二氢-7H-二苯并[a,g]咔唑-7-基)乙基4-甲基苯磺酸盐快速衍生化。采用响应面法（RSM）结合Box-Behnken设计（BBD）对影响萃取效率和衍生化产率的主要实验参数进行了研究和优化。检测限（LOD）和定量限（LOQ）分别在0.95 - 1.36 ng mL(-1)和3.17 - 4.55 ng mL(-1)范围内。在最佳条件下，该方法已成功应用于六种不同中药材中三萜酸的分析。
