Ramaiya A, Karnes H T
Department of Pharmacy and Pharmaceutics, Medical College of Virginia, Virginia Commonwealth University, Richmond 23298-980533, USA.
J Chromatogr B Biomed Sci Appl. 1997 Mar 28;691(1):119-29. doi: 10.1016/s0378-4347(96)00435-5.
Simultaneous quantitation of paroxetine and serotonin in rat brain microdialysate is presented as a means to study the neuropharmacokinetics and neuropharmacodynamics of paroxetine, a selective serotonin reuptake inhibitor. In order to achieve this objective, a single-pump column-switching technique was developed. Optimization of the mobile phase in terms of the concentration of ion-pairing agent, pH of mobile phase, temperature of the stationary phase and concentration of organic modifier was investigated and a single mobile phase was developed for both separations. The design was such that the switching valve employed column I (50 mm length) and column II (250 mm length) in series in position A. At 15.3 min, the valve was switched to position B, in which the flow of the mobile phase was directed only through the short column (column I). A flow gradient program was used to increase the flow-rate from 0.125 ml/min to 0.4 ml/min, which enabled a reduction in total analysis time to less than 20 min. The limits of detection for serotonin and paroxetine were 6 fmol and 300 fmol, respectively. The accuracy of the method demonstrated percent differences from spiked samples that were within 12.5% and the precision was found to be within 10% R.S.D.
本文介绍了一种同时定量大鼠脑微透析液中帕罗西汀和血清素的方法，以此来研究选择性血清素再摄取抑制剂帕罗西汀的神经药代动力学和神经药效学。为实现这一目标，开发了一种单泵柱切换技术。研究了流动相在离子对试剂浓度、流动相pH值、固定相温度和有机改性剂浓度方面的优化，并为两种分离开发了单一流动相。设计方案是，切换阀在位置A时将柱I（50 mm长）和柱II（250 mm长）串联。在15.3分钟时，阀切换到位置B，此时流动相仅通过短柱（柱I）。采用流动梯度程序将流速从0.125 ml/min提高到0.4 ml/min，从而使总分析时间缩短至不到20分钟。血清素和帕罗西汀的检测限分别为6 fmol和300 fmol。该方法的准确度表明，加标样品的百分比差异在12.5%以内，精密度在10%相对标准偏差以内。
