高效液相色谱法快速简便测定血清中的强力霉素。在微粒药物递送系统中的应用。

Rapid and simple determination of doxycycline in serum by high-performance liquid chromatography. Application to particulate drug delivery systems.

作者信息

Ruz Noelia, Zabala Maider, Kramer M Gabriela, Campanero M Angel, Dios-Viéitez M Carmen, Blanco-Príeto María J

机构信息

Departamento de Farmacia y Tecnología Farmacéutica, Facultad de Farmacia, Universidad de Navarra, C/Irunlarrea 1, 31080 Pamplona, Spain.

出版信息

J Chromatogr A. 2004 Mar 26;1031(1-2):295-301. doi: 10.1016/j.chroma.2003.12.028.

DOI:10.1016/j.chroma.2003.12.028

PMID:15058596

Abstract

A simple, rapid and sensitive reversed-phase high-performance liquid chromatographic (HPLC) method for the measurement of doxycycline concentrations in both drug delivery systems (DDS) and serum extracted from mice after intraperitoneal (free drug) and intravenous (doxycycline administered in DDS) administration, has been developed. For the analysis of doxycycline in DDS, a known amount of particles was dissolved in chloroform and, after precipitating the polymer with methanol, the drug was assessed in the supernatant. For doxycycline quantification in microsamples of serum, proteins were precipitated with acetonitrile before chromatographic analysis. After centrifugation, the supernatant was mixed with a mixture of methanol and acetic acid (1:1) for analysis. The samples were chromatographed on a narrow-bore C18 column (Alltech Alltima 150 mm x 2.1 mm) using a mobile phase with 55% acetic acid (5%), 25% acetonitrile and 20% methanol. Doxycycline was detected 347 nm and the run time was 10 min. Linearity was confirmed in the concentration range 0.4-80 microg/ml for doxycycline quantification in serum and from 1 to 800 microg/ml for doxycycline extracted from DDS samples.

摘要

已开发出一种简单、快速且灵敏的反相高效液相色谱（HPLC）方法，用于测定腹腔注射（游离药物）和静脉注射（药物递送系统中给予的多西环素）后小鼠药物递送系统（DDS）和血清中的多西环素浓度。对于DDS中多西环素的分析，将已知量的颗粒溶解于氯仿中，用甲醇使聚合物沉淀后，在上清液中评估药物。对于血清微量样品中多西环素的定量，在色谱分析前用乙腈沉淀蛋白质。离心后，将上清液与甲醇和乙酸（1:1）的混合物混合进行分析。样品在窄孔C18柱（Alltech Alltima 150 mm×2.1 mm）上进行色谱分析，流动相为含55%乙酸（5%）、25%乙腈和20%甲醇的溶液。在347 nm处检测多西环素，运行时间为10分钟。血清中多西环素定量的线性范围为0.4 - 80 μg/ml，从DDS样品中提取的多西环素的线性范围为1 - 800 μg/ml。