使用自动柱前衍生化、高效液相色谱和荧光检测法从骨样本中提取和测量帕米膦酸盐。

Extraction and measurement of pamidronate from bone samples using automated pre-column derivatization, high-performance liquid chromatography and fluorescence detection.

作者信息

King L E, Vieth R

机构信息

Department of Clinical Biochemistry, University of Toronto, Ont., Canada.

出版信息

J Chromatogr B Biomed Appl. 1996 Apr 12;678(2):325-30. doi: 10.1016/0378-4347(95)00531-5.

DOI:10.1016/0378-4347(95)00531-5

PMID:8738038

Abstract

A method for the determination of 3-amino-1-hydroxylpropylidene-1, 1-bisphosphonic acid (pamidronate) in bone samples is described. This method combines and modifies parts of previous procedures. Pamidronate is extracted from finely ground bone with dilute hydrochloric acid. Amine-containing contaminants are removed by co-precipitation of pamidronate with calcium. Excess calcium is removed with EDTA and an ion-exchange resin. Pamidronate is automatically derivatized at the primary amine and quantified by high-performance liquid chromatography with fluorescence detection. The method assay was linear in the concentration range 7.5-600 ng/mg bone (20-100 pmol/mg). The imprecision for repeat analyses were 16.5 and 7.8%, at pamidronate levels of 7.5 and 600 ng/mg bone, respectively. The method has been used to analyze bone samples from pharmacokinetic animal studies involving both acute and chronic dosages.

摘要

本文描述了一种测定骨样品中3-氨基-1-羟丙基亚基-1,1-二膦酸（帕米膦酸）的方法。该方法结合并改进了先前方法的部分内容。用稀盐酸从细磨的骨中提取帕米膦酸。通过帕米膦酸与钙的共沉淀去除含胺污染物。用乙二胺四乙酸（EDTA）和离子交换树脂去除过量的钙。帕米膦酸在伯胺处自动衍生化，并通过带荧光检测的高效液相色谱法定量。该方法在7.5 - 600 ng/mg骨（20 - 100 pmol/mg）的浓度范围内呈线性。在帕米膦酸水平分别为7.5和600 ng/mg骨时，重复分析的不精密度分别为16.5%和7.8%。该方法已用于分析涉及急性和慢性剂量的药代动力学动物研究中的骨样品。