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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 a new aconitine aconitine, benzoyl aconitine base in Wuqi Chifengsan tablets (including Radix Aconiti Kusnezoffii, Radix Notoginseng, Radix Ginseng, Artemisia selengensis, and nine herbs with windproofness) Determination of benzoyl aconitine and hypaconitine by HPLC method. Methods: Chromatographic conditions were as follows: Hanbon-C18 column (4.6 mm × 250 mm, 5 μm), mobile phase of acetonitrile-tetrahydrofuran (25:15) L with glacial acetic acid (0.5 mL) (B) at a flow rate of 1.0 m L · min-1. The column temperature was 30 ℃ and the detection wavelength was set at 232 nm. Results: The four alkaloids were well separated and the linear relationship was obtained between the mass concentration and the peak area of the four alkaloids (r> 0.999 0). The recoveries of the four alkaloids were 101.10% (RSD 2.1%) and 101.09% RSD 2.2%), 102.04% (RSD 1.6%), and 97.83% (RSD 2.7%). The lowest detection limits were 3.4, 1.7, 2.2 and 0.8 ng respectively. Conclusion: The HPLC method is stable, reliable and simple. It can be used for the simultaneous determination of benzoyl aconitine, benzoyl aconitine, benzoyl aconitine and Aconitine content.