采用固相萃取、柱前衍生化和反相高效液相色谱法测定大鼠血浆中的5HT1a激动剂U-89968E。
Determination of U-89968E, a 5HT1a agonist in rat plasma using solid-phase extraction, precolumn derivatization and reversed-phase high-performance liquid chromatography.
作者信息
Rees S A, Austin P M
机构信息
Pharmacia and Upjohn, West Sussex, UK.
出版信息
J Pharm Biomed Anal. 1997 Mar;15(6):739-48. doi: 10.1016/s0731-7085(96)01892-4.
A selective and sensitive HPLC method was developed for the determination of U-39968E in rat plasma. The assay involved solid-phase extraction of the analyte and the internal standard and precolumn derivatization with cyclohexane-1,3-dione reagent before injection on to the HPLC column. The samples were chromatographed on a Spherisorb S5 CN column (25 cm x 4.6 mm i.d.) with a mobile phase containing acetonitrile-trifluoroacetic acid-water (17:0.2:83, v/v/v) at a flow rate of 1.5 ml min-1. The column eluent was monitored by flourescence detection with excitation at 272 nm and emission at 320 nm. The assay is linear over the range 4-759 ng ml-1. The relative standard deviation at the limit of quantification, 4 ng ml-1, was 7.1%. This method was successfully applied to the determination of U-89968E in rat plasma during pharmacokinetic studies.
建立了一种选择性和灵敏的高效液相色谱法用于测定大鼠血浆中的U - 39968E。该测定方法包括对分析物和内标进行固相萃取，以及在注入高效液相色谱柱之前用环己烷 - 1,3 - 二酮试剂进行柱前衍生化。样品在Spherisorb S5 CN柱（25 cm×4.6 mm内径）上进行色谱分析，流动相为含乙腈 - 三氟乙酸 - 水（17:0.2:83，v/v/v），流速为1.5 ml min⁻¹。通过荧光检测监测柱洗脱液，激发波长为272 nm，发射波长为320 nm。该测定方法在4 - 759 ng ml⁻¹范围内呈线性。在定量限4 ng ml⁻¹处的相对标准偏差为7.1%。该方法成功应用于药代动力学研究中大鼠血浆中U - 89968E的测定。
Zotero 插件