DETERMINATION OF A CYCLIC HEPTAPEPTIDE, A NOVEL FIBRINOGEN RECEPTOR ANTAGONIST, IN HUMAN PLASMA BY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH AUTOMATED PRECOLUMN DERIVATIZATION, COLUMN SWITCHING AND FLUORESCENCE DETECTION

被引:11
作者
KLINE, WF [1 ]
MATUSZEWSKI, BK [1 ]
HSIEH, JYK [1 ]
机构
[1] MERCK SHARP & DOHME LTD,W POINT,PA 19486
来源
JOURNAL OF CHROMATOGRAPHY-BIOMEDICAL APPLICATIONS | 1992年 / 578卷 / 01期
关键词
D O I
10.1016/0378-4347(92)80221-B
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A sensitive high-performance liquid chromatographic (HPLC) assay for the determination of the cyclic heptapeptide Ac-Cs-Asn-Dtc-Amf-Gly-Asp-Cys-OH (Dtc = beta,beta-dimethylthioproline, Amf = p-aminomethylphenylalanine) in human plasma has been developed. The key steps in the assay include: solid-phase extraction of the drug from plasma, chemical derivatization of the primary amino group with naphthalene-2,3-dicarboxyaldehyde in the presence of N-acetyl-D-penicillane as a nucleophile to form a fluorescent benzo[f]isoindole derivative, and HPLC with column switching to provide the necessary chromatographic separation of the derivative from endogeneous plasma components. The assay has been validated in the concentration range 1-10 ng/ml of plasma.
引用
收藏
页码:31 / 37
页数:7
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