Yu Lishuang, Xu Xueqin, Huang Lu, Lin Jinming, Chen Guonan
Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian 350002, China.
J Chromatogr A. 2008 Jul 11;1198-1199:220-5. doi: 10.1016/j.chroma.2008.05.024. Epub 2008 May 21.
A new rapid and reproducible method using microemulsion electrokinetic chromatography (MEEKC) combining field amplified sample injection and electroosmotic flow suppressant for the analysis of five quinolizidine alkaloids is developed in this paper. For the separation of five quinolizidine alkaloids, a running buffer composed of 1.2% (v/v) 1-butanol, 0.6% (v/v) ethyl acetate and 98.2% (v/v) 1 mM Na(2)B(4)O(7)-2 mM NaH(2)PO(4) buffer solution containing 21 mM sodium cholate (SC) (pH 6.5) was developed. The resolution of the analytes was improved significantly by adding a divalent cation (e.g., Mg(2+)) to the running buffer as an electroosmotic flow modification. In order to analyze trace quinolizidine alkaloids in traditional Chinese herbal medicines, field amplified sample injection (FASI) was applied to increase the detection sensitivity. The detection limits (defined as S/N=3) for the analytes could be as low as 0.0001 microg/mL. This method was applied for the determination of quinolizidine alkaloids in real samples with simple extraction procedures, and the assay results were satisfactory.
本文开发了一种新的快速且可重现的方法,该方法采用微乳液电动色谱法(MEEKC),结合场放大进样和电渗流抑制剂来分析五种喹诺里西啶生物碱。为分离这五种喹诺里西啶生物碱,开发了一种运行缓冲液,其由1.2%(v/v)的正丁醇、0.6%(v/v)的乙酸乙酯和98.2%(v/v)含有21 mM胆酸钠(SC)(pH 6.5)的1 mM Na₂B₄O₇ - 2 mM NaH₂PO₄缓冲溶液组成。通过向运行缓冲液中添加二价阳离子(如Mg²⁺)作为电渗流调节剂,显著提高了分析物的分离度。为了分析中草药中的痕量喹诺里西啶生物碱,采用场放大进样(FASI)来提高检测灵敏度。分析物的检测限(定义为S/N = 3)可低至0.0001 μg/mL。该方法通过简单的提取程序用于实际样品中喹诺里西啶生物碱的测定,测定结果令人满意。