Determination of pamidronate in urine by ion-pair liquid chromatography after derivatization with 1-naphthylisothiocyanate |
| |
| Institution: | 1. Department of Clinical Pharmacy and Toxicology, Leiden University Hospital, PO Box 9600, 2300 RC Leiden, The Netherlands;2. Department of Pharmacy, Antoni van Leeuwenhoekhuis/Slotervaartziekenhuis, Louwesweg 6, 1066 EC Amsterdam, The Netherlands;1. Veterinary Clinic for Obstetrics, Gynecology and Andrology, Justus Liebig University, Giessen, Germany;2. Steroid Research and Mass Spectrometry Unit, Center of Child and Adolescent Medicine, Justus Liebig University, Giessen, Germany;1. Department of Chemistry and Biochemistry, Miami University, Oxford, OH 45056, United States;2. School of Engineering, University of Vermont, Burlington, VT 05405, United States;1. Dipartimento di Chimica, Biologia e Biotecnologie, University of Perugia, Italy;2. Dipartimento di Scienze Agrarie, Alimentari e Ambientali, University of Perugia, Italy;1. Laboratory of Analytical and Bio-Analytical Chemistry, Graduate Division of Pharmaceutical Sciences, University of Shizuoka, 52-1 Yada, Shizuoka, Suruga-Ku, Shizuoka 422-8526, Japan;2. Analytical and Quality Evaluation Research Laboratories, Daiichi Sankyo Co., Ltd., 1-12-1 Shinomiya, Hiratsuka, Kanagawa 254-0014, Japan |
| |
| Abstract: | A sensitive method for the determination of pamidronate disodium (3-amino-1-hydroxypropylidene)bisphosphonate, APD] in urine has been developed and validated. The procedure involves a triple co-precipitation with calcium phosphate, solid-phase extraction on a quaternary ammonium column, derivatization with 1-naphthylisothiocyanate and ion-pair liquid–liquid extraction. From the two reaction products, naphthylthiocarbamyl-APD is converted into the other, naphthylcarbamyl-APD, by an oxidative desulphuration with hydrogen peroxide prior to analysis by ion-pair HPLC and fluorescence detection at 285/390 nm. The method has a coefficient of variation of 7% for the intra-assay precision of 99 ng ml−1 APD and 11% for the inter-assay precision. The lower limit of quantification is 3 ng ml−1 APD in 2.5 ml of human urine. |
| |
| Keywords: | |
| 本文献已被 ScienceDirect 等数据库收录！ |
|
