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机构地区:[1]南方医科大学药学院分子药剂系,广州510515
出 处:《中华中医药杂志》2012年第12期3204-3206,共3页China Journal of Traditional Chinese Medicine and Pharmacy
基 金:国家重点基础研究发展计划(973计划)子课题资助项目(No.2009CB522808)~~
摘 要:目的:建立高效液相色谱(HPLC)同时测定附子及其炮制品在不同提取溶剂中的乌头碱、中乌头碱及次乌头碱3种双酯二萜型生物碱含量的方法。方法:采用Agilent Eclipse plus C18柱(4.6mm×150mm,5μm),以乙腈和碳酸氢铵(10mmol/L,pH=9.8±0.2)作为流动相进行梯度洗脱;流速1mL/min;进样体积200μL;检测波长240nm;柱温30℃。结果:乌头碱、中乌头碱、次乌头碱分离良好,各成分在0.78-50.00μg/mL内均呈良好的线性关系(r>0.999);平均加样回收率(n=6)为91.4-103.4%,RSD在2.41-4.20%。结论:本方法简便、准确、灵敏,可用于附子及其炮制品中乌头碱类化合物的提取以及定量分析,为附子及其炮制品的质量控制奠定基础。Objective: A sensitive HPLC method was used to determine aconitine,mesaconitine,and hypaconitine as target markers in different methanol extracts and pure water extracts of(i) Fuzi,and(ii) processed roots(Radix Aconiti Praeparata).Methods: These alkaloids were separated by C18 column(4.6mm×150mm,5μm) with ingredient elution using a mobile phase consisted of ammonium bicarbonate(10mM,pH=9.8 ± 0.2) and acetonitrile,which was found to be the optimal solvent of the elution systems examined.The detection wavelength was set at 240nm,the flow rate at 1mL/min and the column temperature at 30℃.Results: Calibration curves with UV detection were linear(r0.999) on injection of amounts ranging from 0.78 to 50μg/mL,extraction recovery(n=6) were ranged from 91.4%-103.4% for the three studied alkaloids.Conclusion: A sensitive and specific HPLC method had been developed and successfully applied for analyzing aconitine,mesaconitine and hypaconitine in aqueous media and mixed methanol.It can be used for quantitive control of aconite roots and its processing products.
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