Liu Yan-Ming, Tian Wei, Jia Yu-Xiu, Yue Hai-Yan
College of Chemistry and Chemical Engineering, Xinyang Normal University, Xinyang 464000, People's Republic of China.
Biomed Chromatogr. 2009 Nov;23(11):1138-44. doi: 10.1002/bmc.1235.
A novel method for the determination of ephedra alkaloids (methylephedrine and pseudoephedrine) was developed by electrophoresis capillary (CE) separation and electrochemiluminesence detection (ECL). The use of ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, BMIMBF(4)) improved the detection sensitivity markedly. The conditions for CE separation, ECL detection and effect of ionic liquid were investigated in detail. The two ephedra alkaloids with very similar structures were well separated and detected under the optimum conditions. The limits of detection (signal-to-noise ratio = 3) in standard solution were 1.8 x 10(-8) mol/L for methylephedrine (ME) and 9.2 x 10(-9) mol/L for pseudoephedrine (PSE). The limits of quantitation (signal-to-noise ratio = 10) in human urine samples were 2.6 x 10(-7) mol/L for ME and 3.6 x 10(-7 )mol/L for PSE. The recoveries of two alkaloids at three different concentration levels in human urine samples were between 81.7 and 105.0%. The proposed method was successfully applied to the determination of ME and PSE in human urine and the monitoring of pharmacokinetics for PSE. The proposed method has potential in therapeutic drug monitoring and clinical analysis.
建立了一种采用毛细管电泳(CE)分离和电化学发光检测(ECL)测定麻黄生物碱(甲基麻黄碱和伪麻黄碱)的新方法。离子液体(1-丁基-3-甲基咪唑四氟硼酸盐,BMIMBF(4))的使用显著提高了检测灵敏度。详细研究了CE分离条件、ECL检测条件以及离子液体的影响。在最佳条件下,结构非常相似的两种麻黄生物碱得到了很好的分离和检测。标准溶液中的检测限(信噪比=3),甲基麻黄碱(ME)为1.8×10(-8) mol/L,伪麻黄碱(PSE)为9.2×10(-9) mol/L。人尿样中的定量限(信噪比=10),ME为2.6×10(-7) mol/L,PSE为3.6×10(-7 )mol/L。人尿样中两种生物碱在三个不同浓度水平的回收率在81.7%至105.0%之间。该方法成功应用于人尿中ME和PSE的测定以及PSE的药代动力学监测。该方法在治疗药物监测和临床分析方面具有潜力。