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高效液相色谱法结合库仑检测法测定人血清中的去氧肾上腺素。

High-performance liquid chromatographic determination of phenylephrine in human serum with coulometric detection.

作者信息

Vuma V, Kanfer I

机构信息

Biopharmaceutics Research Institute, School of Pharmaceutical Sciences, Rhodes University, Grahamstown, South Africa.

出版信息

J Chromatogr B Biomed Appl. 1996 Apr 12;678(2):245-52. doi: 10.1016/0378-4347(95)00487-4.

DOI:10.1016/0378-4347(95)00487-4
PMID:8738028
Abstract

A high-performance liquid chromatographic method for the determination of phenylephrine (PE) in human serum using coulometric detection is described. PE and internal standard, orciprenaline, were extracted from serum by solid-phase extraction and separation achieved on a coupled column system consisting of two C18 cartridge columns (250 x 4.6 mm I.D. coupled to a shorter 50 x 4.6 mm I.D. column) using a mobile phase of methanol-50 mM phosphate buffer (pH 3.2; 10:90) at 36 degrees C. Dual electrode coulometric detection was used in the "oxidative screen" mode. Calibration curves were linear over the range 0.3-4 ng/ml with a limit of quantification (LOQ) of 0.35 ng/ml. The method has a greater degree of sensitivity, precision and accuracy compared to previously published methods for PE and is suitable for use in pharmacokinetic and bioequivalence studies in humans.

摘要

描述了一种采用库仑检测法测定人血清中去氧肾上腺素(PE)的高效液相色谱方法。通过固相萃取从血清中提取PE和内标奥西那林,使用由两根C18柱(250×4.6 mm内径与一根较短的50×4.6 mm内径柱相连)组成的联用柱系统,在36℃下以甲醇 - 50 mM磷酸盐缓冲液(pH 3.2;10:90)为流动相进行分离。采用双电极库仑检测的“氧化筛选”模式。校准曲线在0.3 - 4 ng/ml范围内呈线性,定量限(LOQ)为0.35 ng/ml。与先前发表的PE检测方法相比,该方法具有更高的灵敏度、精密度和准确度,适用于人体药代动力学和生物等效性研究。

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