Semi-automatic liquid chromatographic analysis of pamidronate in urine after derivatization with 1-naphthylisothiocyanate |
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| Affiliation: | 1. Leiden University Medical Center, Department of Clinical Pharmacy and Toxicology, PO Box 9600, 2300 RC Leiden, The Netherlands;2. Slotervaart Hospital, Faculty of Pharmacy and Pharmacology, 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. 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;1. Department of Food Science and Technology, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, 1000 Ljubljana, Slovenia;2. Centre of Excellence for Integrated Approaches in Chemistry and Biology of Proteins (CipKeBiP), Jamova 39, Ljubljana, Slovenia |
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| Abstract: | An existing sensitive chromatographic assay for pamidronate in urine has considerably been automated. Using the same sample processor, the solid-phase extraction (SPE) was automated separately from the derivatization with 1-naphthylisothiocyanate, the two-fold ion-pair liquid–liquid-extraction and the treatment with hydrogen peroxide for the 2–20 ng/ml concentration range. The automatic procedure was preceded by a triple calcium precipitation and interrupted by evaporation of the SPE eluate under nitrogen. For the 0.5–5 μg/ml concentration range one automatic sequence was used by avoiding evaporation during the sample treatment. In addition to the labour-saving of the semi-automatic procedure, the daily sample-throughput was improved compared to the existing manual assay. Further, the validation showed marginal improvements in the precision, accuracy and lower limit of quantification. |
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