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使用库仑检测法通过灵敏的高效液相色谱法测定生物体液中环苯那敏及其去甲基代谢物去甲环苯那敏。

Sensitive high-performance liquid chromatographic determination of cyclizine and its demethylated metabolite, norcyclizine, in biological fluids using coulometric detection.

作者信息

Walker R B, Kanfer I

机构信息

School of Pharmaceutical Sciences, Rhodes University, Grahamstown, South Africa.

出版信息

J Chromatogr B Biomed Appl. 1995 Oct 6;672(1):172-7. doi: 10.1016/0378-4347(95)00202-t.

DOI:10.1016/0378-4347(95)00202-t
PMID:8590933
Abstract

An accurate, sensitive, selective and reproducible high-performance liquid chromatographic method with coulometric detection for the determination of cyclizine and its inactive demethylated metabolite, norcyclizine, in biological fluids has been developed. The drugs were separated using a custom packed reversed-phase C18 analytical column and phosphate buffer (0.05 M, pH 3)-acetonitrile (7:3) as mobile phase. The dual electrode coulometric detector was operated in the "oxidative-screen" mode with the upstream electrode (detector 1) set at 0.55 V and the downstream electrode (detector 2) set at 0.90 V. Serum and urine samples were prepared for analysis by solid-phase extraction, followed by a simple phase-separation step. The limit of quantitation was 1 ng/ml for both cyclizine and norcyclizine in serum and urine.

摘要

已开发出一种准确、灵敏、选择性好且可重现的高效液相色谱法,并采用库仑检测法来测定生物流体中环苯那敏及其无活性的去甲基代谢物去甲环苯那敏。使用定制填充的反相C18分析柱,以磷酸盐缓冲液(0.05M,pH 3)-乙腈(7:3)作为流动相来分离药物。双电极库仑检测器在“氧化-筛选”模式下运行,上游电极(检测器1)设置为0.55V,下游电极(检测器2)设置为0.90V。血清和尿液样本通过固相萃取制备用于分析,随后进行简单的相分离步骤。血清和尿液中环苯那敏和去甲环苯那敏的定量限均为1 ng/ml。

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