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高效液相色谱法测定人血清中甲硝唑的简单灵敏方法。

Simple and sensitive method for determination of metronidazole in human serum by high-performance liquid chromatography.

作者信息

Galmier M J, Frasey A M, Bastide M, Beyssac E, Petit J, Aiache J M, Lartigue-Mattei C

机构信息

Groupe de Recherche en Biodynamique du Médicament, Laboratoire de Chimie Analytique et de Spectrométrie de Masse, Faculté de Pharmacie, Clermont-Ferrand, France.

出版信息

J Chromatogr B Biomed Sci Appl. 1998 Dec 11;720(1-2):239-43. doi: 10.1016/s0378-4347(98)00443-5.

DOI:10.1016/s0378-4347(98)00443-5
PMID:9892088
Abstract

A simple and sensitive HPLC method for determination of metronidazole in human plasma has been developed. A step of freezing the protein precipitate allowed an efficient separation of aqueous and organic phases minimizing the noise level and improved therefore the limit of quantitation (10 ng ml(-1) using 1 ml of plasma sample). The separation of compounds was performed on a RP 18 column with acetonitrile-aqueous 0.01 M phosphate solution (15:85, v/v) as mobile phase. Detection was performed by UV absorbance at 318 nm. Metronidazole was well resolved from the plasma constituents and internal standard. An excellent linearity was observed between peak-height ratios plasma concentrations over a concentration range of 0.01 to 10 microg ml(-1). Within-day and between-day precision (expressed by relative standard deviation) and accuracy (mean error in per cent) did not exceed 4% between 1 and 10 microg ml(-1) and 8.3 and 7.2% respectively for the limit of quantitation. The method is suitable for bioavailability and pharmacokinetic studies in humans.

摘要

已开发出一种用于测定人血浆中甲硝唑的简单且灵敏的高效液相色谱法。冷冻蛋白质沉淀这一步骤能有效分离水相和有机相,将噪声水平降至最低,从而提高了定量限(使用1 ml血浆样品时为10 ng ml⁻¹)。化合物的分离在RP 18柱上进行,以乙腈 - 0.01 M磷酸盐水溶液(15:85,v/v)作为流动相。通过在318 nm处的紫外吸光度进行检测。甲硝唑与血浆成分和内标物得到了很好的分离。在0.01至10 μg ml⁻¹的浓度范围内,观察到峰高比与血浆浓度之间具有良好的线性关系。在1至10 μg ml⁻¹之间,日内和日间精密度(以相对标准偏差表示)以及准确度(百分比平均误差)分别不超过4%和定量限的8.3%和7.2%。该方法适用于人体生物利用度和药代动力学研究。

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