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作 者:陈冉[1] 彭冰[2] 李德慧[3] 孙科[3] 黄锁义[4]
机构地区:[1]右江民族医学院科学实验中心,广西百色533000 [2]右江民族医学院检验学院,广西百色533000 [3]右江民族医学院基础医学院,广西百色533000 [4]右江民族医学院药学院,广西百色533000
出 处:《中国医药导报》2016年第36期145-148,共4页China Medical Herald
基 金:国家自然科学基金项目(81360684);广西高校桂西地区高发病防治研究重点实验室开放课题(xzdsysyy2015311)
摘 要:目的优化鸡骨草中生物碱的提取工艺,建立相思子碱、下箴刺桐碱的超高效液相色谱(UHPLC)测定方法。方法 以相思子碱、下箴刺桐碱的提取量为指标,采用正交试验设计考察乙醇体积分数、料液比、提取时间、提取次数对提取工艺的影响;色谱条件:Shim-pack XR-ODSⅡ色谱柱(2.0 mm×75 mm,2.2μm);流动相:甲醇-乙腈-水-乙酸-三乙胺(6∶2∶92∶0.2∶0.3);检测波长280 nm;流速0.4 mL/min;进样量2μL;柱温30℃。结果 最佳提取条件为加10倍量45%乙醇,提取时间40 min,超声提取2次;相思子碱和下箴刺桐碱分别在1.49-148.80μg/mL(r=0.9998),0.84-84.20μg/mL(r=0.9998)范围内有良好的线性关系,加样回收率为98.9%、98.2%,RSD均〈2%。结论 本提取方法简单、快速、效率高;测定方法准确、高效;不同产地鸡骨草中相思子碱、下箴刺桐碱含量差异明显,以根部含量最多,其次为茎部,最少的部位是叶子。为鸡骨草药材的有效开发利用和质量控制提供了参考依据。Objective To optimize extraction technology of alkaloids in A brus cantoniensis Hance. Establish UHPLC for the determination of abrine and hypaphorine. Methods With abrine and hypaphorine as index ingredients, orthogonal test was used to investigate the effects of ethanol concentration, solid-liquid ratio, extraction time, extraction times on extraction technology. The analysis was performed on Shim-pack XR-ODS II column (2.0 mm×75 mm, 2.2 μm) with the mobile phase of methanol and acetonitrile - water - acetic acid - triethylamine (6:2:92:0.2:0.3) at a flow rate of 0.4 mL/min. The injection volume was 2 μL. The detection wavelength was 280 nm and the column temperature was 30℃. Results The optimal conditions for the extraction technology were as follows: ultrasonic extraction for two times, each time for 40 min with 10 times the amount of 45% ethanol. Abrine and hypaphorine had good linear relationship within 1.49-148.80 μg/mL (r = 0.9998), 0.84-84.20 μg/mL (r = 0.9998), respectively. The sample recoveries were 98.9% and 98.2% , and RSD was less than 2%. Conclusion This extraction method was simple, rapid and high efficiency. Quantitative determination method was accurate and efficient. It had a obvious difference for contents of abrine and hypaphofine in Abrus cantoniensis Hance from different areas and different parts With root 〉 stem 〉 leaf. The resuit provided a reference for effective development quality control of A brus cantoniensis Hance .
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