钩藤总碱中钩藤碱和异钩藤碱定量方法的建立及稳定性试验

Investigation of rhynchphylla total alkaloids stability and the quantitative determineation of rhyncho-phylline and isorhynchophylline

目的建立钩藤总碱中钩藤碱和异构藤碱的含量测定方法并对其稳定性进行研究。方法采用C18柱(4.6 mm×150 mm,5μm),甲醇∶0.1 mol/L三乙胺溶液(冰醋酸调pH 7.5)44∶56为流动相,流速为1.0 ml/min。检测波长254 nm。比较分别放置在室温、6℃条件下的同一批次2份总碱中钩藤碱、异构藤碱的含量变化。结果钩藤碱进样量在0.020 2～0.101 mg/ml线性关系良好,r=0.999 9;异构藤碱进样量在0.020 6～0.103 mg/ml线性关系良好,r=0.999 9,钩藤碱平均回收率为99.67%,RSD为0.97%;异钩藤碱平均回收率为99.95%,RSD为1.02%。结论建立的方法简便、准确,可作为钩藤总碱的含量测定方法;钩藤碱、异构藤碱不稳定,可随时间延长含量下降,且温度对二者皆有影响,对钩藤碱影响较大。

Objective To establish a method for determination of quantitative of rhynchophylline and isorhynchophylline in rhynchphylla total alkaloids, and to study the stability of them. Methods The column used was C18 （4.6mm×150mm,5 μm）. The mobile phase used was Methanol-0.1 mol/L triethylamine solution （44：56, pH 7.5adjusted by glacial acetic acid）. The detection wavelength was set at 254nm. The flow rate was 1.0 ml/min; the quantitative changes of rhynchophylline and isorhynchophylline of rhynchphylla total alkaloids at room temperature and 6 ℃ were compared. Results The average recovery rate of rhynchophylline and isorhynchophylline was 99.67% and 99.95%, the RSD was 0.97% and 1.02%, respectively. The linear range of rhynchophylline and isorhynchophylline was in 0.020 2-0.101 mg/ml and 0.020 6-0.103 mg/ml. Conclusion The established method is accurate and simple that can be used for the quality control of rhynchphylla total alkaloids. Rhynchophylline and isorhynchophylline are instability, which descend along with the time. The rhynchophylline and isorhynchophylline are effected by temperature, and the former has be more influenced than the later.