HPLC同时测定乌七祛风散片中4种生物碱的含量  

Simultaneous Determination of Four Alkaloids in Wuqi Qufengsan Tablets by HPLC

作　　者：毛坤军 潘以琳[1] 李富强[1] 白钢钢[1] 李祥[1] 陈建伟[1] 

机构地区：[1]南京中医药大学,南京210046

出　　处：《中国实验方剂学杂志》2014年第22期74-77,共4页Chinese Journal of Experimental Traditional Medical Formulae

摘　　要：目的:建立乌七祛风散片(制草乌、三七、断节参、雪上一枝蒿、防风等9味中药组成)中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱和次乌头碱的HPLC测定方法。方法:色谱条件,Hanbon-C18色谱柱(4.6 mm×250 mm,5μm),流动相[乙腈-四氢呋喃(25∶15)](A)-0.1 mol·L-1醋酸铵溶液(每1 000 m L加冰醋酸0.5 m L)(B),流速1.0 m L·min-1,柱温30℃,检测波长232 nm。结果:4种生物碱分离良好,各成分质量浓度与峰面积在测定范围内均呈良好的线性关系(r>0.999 0),加样回收率分别为101.10%(RSD 2.1%),101.09%(RSD 2.2%),102.04%(RSD 1.6%),97.83%(RSD 2.7%),最低检测限分别为3.4,1.7,2.2,0.8 ng。结论:该HPLC方法稳定可靠、简便易行,可用于同时测定乌七祛风散片中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱和次乌头碱含量。Objective： To establish an HPLC method for simultaneous determination of benzoylmesaconine,benzoylaconine,benzoylhypacoitine and hypaconitine in Wuqi Qufengsan tablets. Method：The assay was performed on a Hanbon-C18（ 4. 6 mm × 250 mm,5 μm）,mobile phase consisted of acetonitriletetrahydrofuran（ 25∶ 15,phase A）-0. 1 mol·L^-1ammonium acetate（ containing 0. 5 m L glacial acetic acid per1 000 m L,phase B） with gradient elution at the flow rate of 1. 0 m L·min^-1,column temperature was 30 ℃,and the detection wavelength was at 235 nm. Result： Excellent chromatographic separation was achieved for four studied alkaloids with good linearity（ r〉 0. 999 0）,the average recoveries were 101. 10%（ RSD 2. 1%）,101. 09%（ RSD 2. 2%）,102. 04%（ RSD 1. 6%）,97. 83%（ RSD 2. 7%）. The limits of detection were3. 4,1. 7,2. 2and 0. 8 ng respectively. Conclusion： This method was simple, accurate and reproducible, it can be used to determine the content of benzoylmesaconine,benzoylaconine,benzoylhypacoitine and hypaconitine in Wuqi Qufengsan tablets.

关 键 词：乌七祛风散片剂 苯甲酰新乌头原碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 次乌头碱 

分 类 号：R284.1[医药卫生—中药学]