PREPARATIVE SEPARATION AND PURIFICATION OF ALKYLAMIDES FROM ZANTHOXYLUM BUNGEANUM MAXIM BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY
PREPARATIVE SEPARATION AND PURIFICATION OF ALKYLAMIDES FROM ZANTHOXYLUM BUNGEANUM MAXIM BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY
复制标题
高速逆流色谱法制备分离纯化花椒中烷基酰胺类化合物
DOI：
10.1080/10826076.2011.593219
复制
发表时间：
2011-01-01
影响因子：
1.3
通讯作者：
Sun, Baoguo
中科院分区：
文献类型：
--
作者：
Wang, Shi;Xie, Jianchun;Sun, Baoguo
采用高速逆流色谱法（HSCCC）对花椒皮提取物中刺激性成分烷基酰胺进行了制备分离纯化。下相为正己烷-乙酸乙酯-甲醇-水（7:3:5:5,v/v），流速为1.5 mL。min(-1)，转速为850转/分，1.0 g提取液在2小时内一次提取得到纯度为98.0%的烷基酰胺0.19 g。通过质谱、红外光谱和1h NMR分析，确定产物为羟基- α -三酚、羟基- β -三酚和羟基-epsilon-三酚。以HSCCC产品为外标，测定提取液中烷基酰胺的含量为21.41%，其中羟基- α -三酚、羟基- β -三酚、羟基- ε -三酚的含量分别为15.69%、4.76%、0.96%。
High-speed counter-current chromatography (HSCCC) was successfully applied to preparative isolation and purification of alkylamides, the tingling-taste components, from pericarp extract of Zanthoxylum bungeanum Maxim (Dahongpao). With the lower phase of n-hexane-ethyl acetate-methanol-water (7: 3: 5: 5, v/v) eluted at a flow rate of 1.5 mL . min(-1), and the revolution speed at 850 rpm, 0.19 g of alkylamides in purity of 98.0% by the relative peak area of HPLC was obtained from 1.0 g of extract in one run within 2 hr. On the basis of MS, IR, and 1 H NMR analysis, the product of alkylamides was confirmed to be composed of hydroxy-alpha-sanshool, hydroxy-beta-sanshool, and hydroxy-epsilon-sanshool. Furthermore, using the HSCCC product as external standard, alkylamide in the extract was determined to be in total of 21.41%, among which hydroxy-alpha-sanshool, hydroxy-beta-sanshool, and hydroxy-epsilon-sanshool were in 15.69%, 4.76%, and 0.96%, respectively.