Irth H, Tocklu R, Welten K, de Jong G J, Brinkman U A, Frei R W
Department of Analytical Chemistry, Free University, Amsterdam, The Netherlands.
J Chromatogr. 1989 Jul 21;491(2):321-30. doi: 10.1016/s0378-4347(00)82850-9.
A method was developed for the determination of 3'-azido-3'-deoxythymidine (AZT) in plasma. The method is based on the trace enrichment of AZT on a pre-column packed with a silver-loaded thiol stationary phase at pH 11.6. On-line desorption to the reversed-phase liquid chromatographic system is performed by injecting a plug of 50 microliters of 1 M perchloric acid on the silver (I)-thiol pre-column. Two different sample pretreatment methods - protein precipitation with perchloric acid and on-line clean-up via a polymeric PRP-1 pre-column - were applied for the determination of AZT in human plasma. The latter method allows the direct injection of plasma samples into the analytical system and can therefore easily be automated. With both methods detection limits in the order of 10(-8) M AZT were obtained after preconcentration of 1.0 ml of plasma, using UV detection at 267 nm.
开发了一种测定血浆中3'-叠氮-3'-脱氧胸苷（AZT）的方法。该方法基于在pH 11.6条件下，AZT在填充有负载银硫醇固定相的预柱上进行痕量富集。通过在银（I）-硫醇预柱上注入50微升1 M高氯酸塞子，实现向反相液相色谱系统的在线解吸。应用两种不同的样品预处理方法——用高氯酸沉淀蛋白质和通过聚合物PRP-1预柱进行在线净化——来测定人血浆中的AZT。后一种方法允许将血浆样品直接注入分析系统，因此可以很容易地实现自动化。使用这两种方法，在对1.0毫升血浆进行预浓缩后，采用267纳米的紫外检测，获得了约10^(-8) M AZT的检测限。
