摘要
目的建立优化钩藤药材中钩藤碱的提取及含量测定方法。方法采用甲醇冷浸超声法处理钩藤药材,Diamonsil C18(250mm×4.6mm,5μm)色谱柱,流动相及梯度:甲醇∶0.01mol/L醋酸铵缓冲液(氨水调pH=6.0)0～20min内比例由25∶75递增至50∶50;流速:1.0ml/min;柱温:25℃;检测波长:245nm;进样量:20μl。结果钩藤碱在0.25～64.0μg/ml范围内线性良好,回归方程为y=3.64×104x-2.13×104(r=0.9995),相对回收率为95.95%～114.40%,重复性试验RSD为6.50%,稳定性试验钩藤碱高、中、低浓度溶液室温5d内RSD为4.62%、2.65%和4.58%。结论本测定方法准确可靠,重复性好,可应用于钩藤药材中钩藤碱含量的测定。
Objective To establish and optimize a method to extract and determine rhynchophylline in a traditional Chinese herb,Ramulus Uncariae cum Uncis. Methods Cold maceration with methanol and supersonic extraction was used to treat the medical material. Chromatography was performed on a Diamonsil C18 column （250 mm×4.6 mm,5 μm）. Gradient elution was employed with a mobile phase consisting of methanol （solution A） and ammonium acetate buffer （0.01 mol/L,pH 6.0 adjusted by ammoniae aqua,solution B） as follows： A∶B from 25∶75 to 50∶50 from 0 to 20 min. The flow rate of the mobile phase was 1.0 ml/min and the column was maintained at 20 ℃. The detector was monitored at 245 nm. Results The calibration curve was linear among the concentration range of 0.25 to 64.0 μg/ml （y=3.64×104x-2.13×104,r=0.999 5） and the relative recovery ranged from 95.95% to 114.4%. The relative standard deviation （RSD） of the reproducibility test was 6.50% and of the stability test was 4.62%,2.65% and 4.58% from the high density to the low. Conclusion Our method is accurate,reliable and with good reproducibility,and it can be used for determining rhynchophylline in Ramulus Uncariae cum Uncis.
出处
《第三军医大学学报》
CAS
CSCD
北大核心
2010年第14期1539-1541,共3页
Journal of Third Military Medical University
关键词
钩藤
钩藤碱
高效液相色谱法
Ramulus Uncariae cum Uncis
rhynchophylline
high performance liquid chromatography
