代谢物
色谱法
兴奋剂
人血浆
化学
等离子体
高效液相色谱法
生物化学
受体
量子力学
物理
作者
Stephen C. Kasper,Peter L. Bonate,Allyn F. DeLong
出处
期刊:Journal of Chromatography B: Biomedical Sciences and Applications
[Elsevier]
日期:1995-07-01
卷期号:669 (2): 397-403
被引量:1
标识
DOI:10.1016/0378-4347(95)00124-2
摘要
A reversed-phase high-performance liquid chromatographic assay (HPLC) was utilized for monitoring xanomeline (LY246708/NNC 11-0232) and a metabolite, desmethylxanomeline, in human plasma. Xanomeline, desmethylxanomeline and internal standard were extracted from plasm with hexane at basic pH. The organic solvent extract was evaporated to dryness with nitrogen and the dried residue was reconstituted with 0.2 M HCl-methanol (50:50, v/v). A Zorbax CN 150 x 4.6 mm I.D., 5-microns column and mobile phase consisting of 0.5% (5 ml/l) triethylamine (TEA) adjusted to pH 3.0 with concentrated orthophosphoric acid-tetrahydrofuran (THF) (70:30, v/v) produced consistent resolution of analytes from endogenous co-extracted plasma components. Column effluent was monitored at 296 nm/0.008 a.u.f.s. and the assay limit of quantification was 1.5 ng/ml. A linear response of 1.5 to 20 ng/ml was sufficient to monitor plasma drug/metabolite concentrations during clinical trials. HPLC assay validation as well as routine assay quality control (QC) samples indicated assay precision/accuracy was better than +/- 15%.
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