通过用荧光胺进行柱前衍生化、高效液相色谱法和荧光检测法，改进血浆和尿液中双膦酸盐帕米膦酸二钠的测定。

Improved determination of the bisphosphonate pamidronate disodium in plasma and urine by pre-column derivatization with fluorescamine, high-performance liquid chromatography and fluorescence detection.

作者信息

Flesch G, Tominaga N, Degen P

机构信息

Research and Development, Pharmaceuticals Division, Ciba-Geigy Limited, Basle, Switzerland.

出版信息

J Chromatogr. 1991 Jul 17;568(1):261-6. doi: 10.1016/0378-4347(91)80362-g.

DOI:10.1016/0378-4347(91)80362-g

PMID:1770106

Abstract

An improved method for the determination of 1-hydroxy-3-aminopropylidene-1,1-bisphosphonate (pamidronate) in human urine and plasma is described. The procedure is based on a co-precipitation of the bisphosphonates (pamidronate and 6-amino-1-hydroxypentilidene-bisphosphonate, used as internal standard) with calcium phosphate. After centrifugation the precipitate is redissolved in hydrochloric acid, followed by a second precipitation. Then the bisphosphonates are dissolved in ethylenediaminetetraacetic acid, derivatized with fluorescamine, and separated by high-performance liquid chromatography. Using fluorescence detection, the limit of quantitation for pamidronate was 0.8 mumol/l in plasma and 0.7 mumol/l in urine.

摘要

本文描述了一种改进的测定人尿液和血浆中1-羟基-3-氨基亚丙基-1,1-二膦酸盐（帕米膦酸盐）的方法。该方法基于二膦酸盐（帕米膦酸盐和用作内标的6-氨基-1-羟基戊叉二膦酸盐）与磷酸钙的共沉淀。离心后，沉淀物用盐酸重新溶解，然后进行第二次沉淀。然后将二膦酸盐溶解在乙二胺四乙酸中，用荧光胺衍生化，并用高效液相色谱法分离。采用荧光检测，帕米膦酸盐在血浆中的定量限为0.8μmol/L，在尿液中的定量限为0.7μmol/L。