TLC一HPLC法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量

Quantitative Determination of Mesaconitine, Hypaconitine and Aconitine in Xiaohuoluo Pills by TLC-HPLC

采用ＴＬＣ－ＨＰＬＣ法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量。在硅胶Ｇ薄层板上以石油醚（６０～９０℃）－正己烷－醋酸乙酯－无水乙醇－浓氨水（１：２：５：５：０．５）为展开剂，分离提取酯型生物碱，用Ｒｅｓｏｌｖｅ Ｓｐｈｅｒｉｃａｌ Ｓｉｌｉｃａ柱（５μｍ，１５０ｍｍ×３．９ｍｍ），以无水乙醇－０．４％醋酸铵水溶液（９７：３）为流动相进行测定，检测波长２３１ｎｍ，平均回收率：８３．２％（中乌头碱）、９２．１（次乌头碱）、８４．１％（乌头碱）。

This paper reports the determination of mesaconitine、hypaconitine and aconitine in Xiaohuoluo pills by TLC-HPLC. The alkaloids were isolated by TLC with petroleum ether- (60 ～90℃-hexane-ethyl acetate-absolute ethanol-ammonium hydroxide (1:2:5:5: 0.5) as developer, and were then separated and determined by HPLC on Resolve Spherical Silica (5μm) column (150mm×3. 9mm) with absolute ethanol-0.4%ammonium acetate in water (97:3) as mobile phase. The eluent was monitored at 231nm. The average recoveries were: 83. 2% (mesaconitine); 92. l% (hypaconitine); 84. 1% (aconitine).