鸡骨草中生物碱的提取与测定
超高效液相色谱,正交试验
陈冉 彭冰 李德慧[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-ODS Ⅱ色谱柱(2.0 mm×75 mm,2.2 μm);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2 μL;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1.49~148.80 μg/mL(r=0.9998),0.84~84.20 μg/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。
[关键词] 鸡骨草;超声提取法;相思子碱;下箴刺桐碱;超高效液相色谱;正交试验
[中图分类号] R284.2 [文献标识码] A [文章编号] 1673-7210(2016)12(c)-0145-04
[Abstract] Objective To optimize extraction technology of alkaloids in Abrus 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 ......
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