结合阳离子选择性耗尽-扫集的微乳毛细管电泳法测定吴茱萸生物碱

Determination of Evodia rutaecarpa alkaloids by microemulsion electrokinetic chromatography with cation-selective exhaustive injection and sweeping

本文建立了一种毛细管在线富集技术,通过将阳离子选择性耗尽（CSEI）-扫集（sweeping）技术与微乳毛细管电泳相结合,实现了吴茱萸中四种生物碱（1.吴茱萸碱;2.吴茱萸次碱;3.吴茱萸新碱;4.1-甲基-2-十一烷基-4（1H）-喹诺酮）的同时定量检测和分析。通过表面活性剂、有机改性剂、p H等条件的考察得到最佳微乳体系组成为：100 mmol·L^-1SDS,1%（体积比）乙酸乙酯,15%（体积比）正丁醇,15%（体积比）乙腈,2.5%（体积比）甲酸,p H 2.00。通过基底缓冲p H和长度、水塞长度考察,CSEI-sweeping最佳富集条件为,水塞0.5psi水动引入2 s,p H 9.00基底缓冲0.5 psi水动引入90 s,＋10 k V电动进样90 s。富集倍数达到了8-30倍。将此方法应用于实际样品中四种生物碱的定量,获得满意结果。研究结果表明,所建立CSEI-sweeping与MEEKC联用法能快速、准确地应用于吴茱萸四种生物碱的定量分析。

In this study,the determination of the Evodia rutaecarpa alkaloids（ 1. evodiamine; 2. rutaecarpine; 3. evocarpine and 4. 1-Methyl-2-undecyl-4（ 1H）-quinolone） by microemulsion electrokinetic chromatography（ MEEKC） using an on-line enrichment method which coupled cation-selective exhaustive injection（ CSEI） and sweeping were developed. First,to optimize the separations conditions for the alkaloid,the microemulsion compositions（ surfactant,organic modification and solution p H） were examined. The optimum conditions of the microemulsion are 100 mmol·L^-1SDS,1%（ v / v） ethyl acetate,15%（ v / v） 1-butanol,15%（ v / v） acetonitrile,2. 5%（ v / v） formic acid,p H 2. 00. Then,the on-line enrichment method of CSEI-sweeping provide up to a 8 - 30 fold increase in detection sensitivity by examing the p H value and the injection length of basic plug,the length of water plug. After optimization,the optimum CSEI-sweeping condition were as follows： the basic plug of p H 9. 00 is introduced hydrodynamically by pressure at 0. 5 psi for 90 s,the water plug is introduced by pressure at 0. 5 psi for 2 s,and the sample is electrokinetic injected by ＋ 10 k V for 90 s. This method was successfully applied to the quantitation of the four alkaloids in practical samples,and satisfactory results were obtained. The results of these researches shown that CSEI-sweeping MEEKC method could be successfully applied to the detection of the four alkaloids in Evodia rutaecarpa.