天然产物研究与开发 ›› 2019, Vol. 31 ›› Issue (1): 24-29.doi: 10.16333/j.1001-6880.2019.1.004

• 研究论文 • 上一篇    下一篇

HPLC同时测定伤科黄水中6个生物碱的含量

郑芳昊,陈韵姿,雷凯君,李子鸿,李怀国,刘东文,刘效仿*   

  1. 佛山市中医院,佛山 528000
  • 出版日期:2019-01-28 发布日期:2019-01-28
  • 基金资助:

    广东省中医药强省建设专项资金-医院中药制剂开发项目(粤财社[2015]77号);广东省中医药局面上项目(20171260,20181249);佛山市医学类科技攻关项目(2016AB002041)

Simultaneous determination of six alkaloids in Shangkehuangshui by HPLC

ZHENG Fang-hao,CHEN Yun-zi,LEI Kai-jun,LI Zi-hong,LI Huai-guo,LIU Dong-wen,LIU Xiao-famg*   

  1. Foshan Hospital of TCM,Foshan 528000,China
  • Online:2019-01-28 Published:2019-01-28

摘要: 建立HPLC同时测定伤科黄水中6个生物碱的方法。采用XBridge C18色谱柱(3.5 μm,2.1 mm×100 mm),柱温35 ℃,测定波长280 nm,以0.1%磷酸溶液(每100 mL加0.3 g十二烷基苯磺酸钠)(A)-乙腈-水-磷酸-十二烷基苯磺酸钠(90∶10∶0.1∶0.3)(B)为流动相,进行梯度洗脱(0~30 min,B%:35~70;30~31 min,B%:70~35;31~40 min,B%:35)。经方法学验证,黄柏碱、药根碱、表小檗碱、黄连碱、巴马汀、小檗碱等共6个生物碱分离情况良好,在测定时间段内无明显干扰峰;加样回收率均在95%~115%之间,RSD%均小于5%;精密度RSD%均小于5%;在测定浓度范围内(1~50 μg/mL)线性关系良好,相关系数(R2)大于0.999。3个不同批次供试品的测定结果较一致。本研究建立的HPLC分析方法可用于同时测定伤科黄水中6个生物碱的含量。

关键词: 伤科黄水, 高效液相色谱, 黄柏碱, 药根碱, 表小檗碱, 黄连碱, 巴马汀, 小檗碱

Abstract: This research was aimed to establish a quantitative analysis of multi-components by HPLC for the simultaneous determination of six alkaloids (phellodendrine,jatrorrhizine,epiberberine,coptisine,palmatine,and berberine) in Shangkehuangshui.An HPLC method was established to determine the six alkaloids.The determination was performed on XBridge C18(3.5 μm,2.1 mm×100 mm) column with A:water -0.1% phosphoric acid (adding 0.3 g sodium dodecyl sulfate per 100 mL,gradient elution) and B:acetonitrile (90)-water (10)-0.1% phosphoric acid (adding 0.3 g sodium dodecyl sulfate per 100 mL,gradient elution) as mobile phase at the flow rate of 1.0 mL/min,0-30 min (B%:35-70),30-31 min (B%:70-35),31-40 min (B%:35).The detection wavelength was set at 280 nm.The column temperature was 35 ℃.Under the chromatographic conditions,six alkaloids were well separated.The linear range of six alkaloids were 1-50 μg/mL (R2>0.999).RSDs of precision,stability and reproducibility tests were all lower than 5%.The stability of the sample solution was good within 24 hours after preparation.The average recoveries were 95%-115%.The method is feasible and accurate for the simultaneous determination of the six alkaloids in Shangkehuangshui.

Key words: Shangkehuangshui, high performance liquid chromatography, phellodendrine, jatrorrhizine, epiberberine, coptisine, palmatine, berberine

中图分类号: 

R917