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作 者:刘明[1] 汤建林[1] 胡岚岚[1] 周世文[1]
机构地区:[1]第三军医大学新桥医院临床药理基地,重庆400037
出 处:《第三军医大学学报》2010年第14期1539-1541,共3页Journal of Third Military Medical University
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.
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