Riley C M, Sternson L A, Repta A J
J Chromatogr. 1983 Aug 12;276(1):93-102. doi: 10.1016/s0378-4347(00)85069-0.
A sensitive and highly specific assay for riboxamide (TCAR) in human and canine plasma is described. The specificity of the procedure is derived from the method of sample preparation and a high-performance liquid chromatographic separation which utilizes the different selectivities of two columns. Partial separation of TCAR from plasma is achieved on a solvent-generated anion exchanger with silica gel as the solid support. The separation is completed by switching the eluent fraction containing TCAR from the first column to a second solvent-generated anion exchanger which has ODS-silica as its support. The relationship between the amount of drug injected and its peak height was linear over wide ranges of concentrations (0-10 micrograms/ml) and injection volumes (20-200 microliter). The limit of detection for TCAR in plasma was 40 ng/ml which can be detected by injecting 200 microliter of processed plasma. The recoveries from plasma were 100.2 +/- 0.9% and 101.3 +/- 2.3% when spiked at the 10 and 1 microgram/ml levels, respectively. The applicability of the method to pharmacokinetic studies was demonstrated by following the plasma levels of TCAR after intravenous administration in the dog.
本文描述了一种用于测定人和犬血浆中利波酰胺（TCAR）的灵敏且高度特异的分析方法。该方法的特异性源于样品制备方法以及高效液相色谱分离，后者利用了两根色谱柱不同的选择性。以硅胶为固体支持物的溶剂生成型阴离子交换柱可实现TCAR与血浆的部分分离。通过将含有TCAR的洗脱液部分从第一根色谱柱切换至以ODS-硅胶为支持物的第二根溶剂生成型阴离子交换柱来完成分离。在所研究的宽浓度范围（0 - 10微克/毫升）和进样体积范围（20 - 200微升）内，进样药物量与其峰高之间呈线性关系。血浆中TCAR的检测限为40纳克/毫升，通过进样200微升处理后的血浆即可检测到。当分别在10微克/毫升和1微克/毫升水平加样时，血浆回收率分别为100.2±0.9%和101.3±2.3%。通过跟踪犬静脉注射后血浆中TCAR的水平，证明了该方法在药代动力学研究中的适用性。
