高效液相色谱法测定血清中3-(5-环丙基-1,2,4-恶二唑-3-基)-5-(1-甲基乙基)咪唑并[1,5-a]喹喔啉-4(5H)-酮

Determination of 3-(5-cyclopropyl-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)imidazo[1, 5-a]quinoxalin-4(5H)-one in serum by high-performance liquid chromatography.

作者信息

Zhong W Z

机构信息

Drug Metabolism Research, Upjohn Company, Kalamazoo, MI 49001.

出版信息

J Chromatogr. 1991 Feb 15;563(2):427-34. doi: 10.1016/0378-4347(91)80052-e.

DOI:10.1016/0378-4347(91)80052-e

PMID:2056007

Abstract

A high-performance liquid chromatographic assay with solid-phase extraction (SPE) for the rapid and sensitive quantitation of 3-(5-cyclopropyl-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)imidazo[1, 5-a]quinoxalin-4(5H)-one (I, U-78875) in serum is described. The validation results indicated that the present method had excellent intra- and inter-assay precision (less than or equal to 9.5%, mean +/- S.D. = 3.9 +/- 3.0%, n = 25) and accuracy (less than or equal to 10.0%, mean +/- S.D. = 3.0 +/- 2.9%, n = 25), as well as improved sensitivity (2 ng ml, using a 100-microliters injection). Each chromatographic run is only 10 min and the organic solvent for the extraction of I and internal standard (U-82217) from serum was only 300 microliters. The application results obtained from the SPE method were in good agreement with the advanced automated sample preparation method.

摘要

本文描述了一种采用固相萃取（SPE）的高效液相色谱法，用于快速、灵敏地定量测定血清中的3-(5-环丙基-1,2,4-恶二唑-3-基)-5-(1-甲基乙基)咪唑并[1,5-a]喹喔啉-4(5H)-酮（I，U-78875）。验证结果表明，本方法具有出色的批内和批间精密度（小于或等于9.5%，平均值±标准差 = 3.9±3.0%，n = 25）和准确度（小于或等于10.0%，平均值±标准差 = 3.0±2.9%，n = 25），以及更高的灵敏度（2 ng/ml，进样量为100微升）。每次色谱运行仅需10分钟，从血清中萃取I和内标（U-82217）的有机溶剂仅需300微升。SPE方法的应用结果与先进的自动样品制备方法高度一致。