钩藤药材中钩藤碱含量测定方法的建立

目的：建立钩藤药材钩藤碱含量HPLC测定方法。方法：分别对HPLC的色谱柱、流动相、检测波长等色谱条件进行摸索,对样品索式、回流和超声提取方法进行摸索,并采用正交设计的方法考察超声提取的药材破碎度、溶剂浓度、溶剂量和时间。结果：HPLC色谱条件为色谱柱：Gemini C18柱（4.6 mm×250 mm,5μm）,流动相∶甲醇—水（含0.002 mol/L三乙胺,冰乙酸调pH至7.5）（64∶36）,流速：1.0 mL/min,检测波长：254 nm。样品供试液制备方法为：药材破碎度为过60目筛的粉末,提取溶剂为75%甲醇,溶剂加入量为15 mL,超声处理40 min。该方法钩藤碱在0.020 9-1.672 0μg范围内有良好线性关系,平均回收率为98.96%,RSD=0.69%（n=6）。结论：建立的含量测定方法简易、准确,可作为钩藤药材钩藤碱含量测定方法。

ESTABLISHMENT OF DETERMINATION OF RHYNCHOPHYLLINE IN RAMULUS UNCARIAE CUM UNCIS

Objective：To establish the HPLC method for determination rhynchophylline in a traditional Chinese herb,Ramulus Uncariae cum Uncis.Methods：The chromatography column and flow phase,the wavelength of HPLC,the soxhlet extraction process,circumfluence distillation,supersonic extraction on rhynchophylline extraction were reseached.Then the effect of fragmentation degree of medicinal solvent concentration,solvent inventory and extraction duration were studied by the orthogonal design.Results：HPLC chromatographic condition：Gemini C18 column（4.6 mm×250 mm,5 μm）.The mobile phase consisted of methanol-0.002 mol/L triethylomine solution（adjust pH to 7.5 with acetic acid）（64∶36） at the flow of 1.0 mL/min,and the detection wavelength was 254 nm.The method to prepare the sample preparation： the fragmentation degree was 60 mesh,extraction solvent was methanol of 75%,solvent inventory was 15 mL,ultrasonic reaction time was 40 min.The standard curve was linear in 0.020 9-1.672 0 μg.The average recovery and RSD were 98.96% and 0.69%;respectively（n=6）.Conclusion：The method is simple and accurate.It can determine the content of rhynchophylline in Ramulus Uncariae cum Uncis.