微乳电动色谱-激光诱导荧光检测法快速分离测定麻黄碱和伪麻黄碱  

Microemulsion Electrokinetic Chromatography with Laser-Induced Fluorescence Detection for Rapid Separation and Determination of Ephedrine and Pseudoephedrine

作　　者：王卫平[1] 王树民[1] 罗智[1] 胡之德[1] 

机构地区：[1]兰州大学化学化工学院,兰州730000

出　　处：《分析化学》2007年第3期382-385,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.20275014)

摘　　要：以5-（4,6-三氯-s-三嗪基-2-氨基）荧光素为衍生试剂,建立了一种微乳电动色谱-激光诱导荧光检测法分析麻黄碱和伪麻黄碱的新方法。经过实验条件的优化,使用50mmol/L硼砂,5%微乳液（V/V）（微乳液组成（W/W）3.24%正己烷,3.24%SDS,26.44%正丁醇,57.08%水）,14%乙腈（V/V）作为运行缓冲溶液,电压22.5kV,温度为25℃条件下,11min内可实现基线分离。分析物的峰高与浓度（2.5-75μg/L）之间存在较好的线性关系,相关系数为0.9915（麻黄碱）和0.9981（伪麻黄碱）;检出限分别为2.39×10^-3和3.85×10^-3μg/L。将该法成功用于麻黄及其制剂中两种生物碱的分析,回收率在92.0%-108.4%之间。A rapid microemulsion electrokinetic chromatography （MEEKC） with laser-induced fluorescence （LIF） detection method for the analysis of ephedrine （E） and pseudoephedrine （PE） after derivatizated by 5- （4,6-dichloro-s-triazin-2-ylamino） fluorescein （DTAF） was proposed. After a series of optimization, the baseline separation of the two alkaloids could be obtained in less than 11 min with a running buffer consisting of 50 mmol/L borate sodium, 5% （WV） microemulsion （n-heptane （3.24%, W/W）, SDS （3.24%, W/W）, n-butanol （26.44%, W/W） and distilled water （57.08%, W/W）, 14% acetonitrile, and a voltage of 22.5 kV, a temperature of 25 ℃. A linear relationship for E and PE was obtained in the range of 2.5 - 75 μg/L （correlation coefficients： 0. 9915 for E and 0. 9981 for PE）, and the detection limits for E and PE were 2.39 × 10^-3 μg/L, 1.09 × 10 -3 μg/L, respectively. The proposed method was applied to the analysis of the two alkaloids in ehpedra herb and its preparations with recoveries in the range of 92.0% -108.4%.

关 键 词：微乳电动色谱 激光诱导荧光检测 5-(4 6-三氯十三嗪基-2-氨基)荧光素 麻黄碱 伪麻黄碱 

分 类 号：O657.3[理学—分析化学]