Castro-Puyana María, Lammers Ivonne, Buijs Joost, Gooijer Cees, Ariese Freek
Department of Biomolecular Analysis and Spectroscopy, Laser Centre Vrije Universiteit Amsterdam, Amsterdam, The Netherlands.
Electrophoresis. 2010 Dec;31(23-24):3928-36. doi: 10.1002/elps.201000352.
A new CE detection method was developed for the chiral drug bupropion (a second-generation antidepressant), based on phosphorescence both in the direct and in the sensitized mode using pulsed laser excitation at 266 nm. Electrokinetic chromatography using 5 mM sulfated-α-CD as chiral selector in 25 mM phosphate buffer at pH 3 allowed the separation of bupropion enantiomers with a high chiral resolution (Rs>3). In the sensitized phosphorescence detection mode, excitation energy is transferred from the analyte to an acceptor (1-bromo-4-napthhalenesulfonic acid or biacetyl) followed by time-resolved phosphorescence detection under deoxygenated buffer conditions. Using 2 × 10(-4) M biacetyl as the acceptor an LOD of 2 × 10(-7) M was obtained for each enantiomer, about 40 times better than in the direct mode. Under these separation conditions, no significantly different phosphorescence lifetimes (measured on-line) were obtained for the two bupropion enantiomers. The suitability of the method was demonstrated with the quantification of bupropion in a pharmaceutical formulation and its determination in a spiked urine sample.
基于在266 nm处使用脉冲激光激发的直接磷光和敏化磷光模式,开发了一种用于手性药物安非他酮(第二代抗抑郁药)的新型毛细管电泳检测方法。在pH 3的25 mM磷酸盐缓冲液中使用5 mM硫酸化-α-环糊精作为手性选择剂的电动色谱法能够以高的手性分辨率(Rs>3)分离安非他酮对映体。在敏化磷光检测模式下,激发能量从分析物转移到受体(1-溴-4-萘磺酸或双乙酰),然后在脱氧缓冲液条件下进行时间分辨磷光检测。使用2×10(-4)M双乙酰作为受体,每种对映体的检测限为2×10(-7)M,比直接模式下约好40倍。在这些分离条件下,两种安非他酮对映体的磷光寿命(在线测量)没有显著差异。该方法的适用性通过药物制剂中安非他酮的定量以及加标尿液样品中的测定得到了证明。