Rapid Determination of Bisphosphonates by Ion Chromatography with Indirect UV Detection

Abstract

Rapid methods for etidronate, clodronate, pamidronate, and alendronate assays are presented. The methods are based on ion chromatography with indirect UV detection, which avoids the need for chemical derivatization procedures. Each compound is analyzed on an individual basis. There is no need for having separation among these analytes because the aim of the proposed methods is to analyze each compound separately either in bulk material or pharmaceuticals. Phenosphere (150 x 2.0-mm, 5 microm) and Sphereclone (250 x 2.0-mm, 5 microm) anion exchange columns were employed with sodium citrate (20mM) as the mobile phase. The methods are simple, rapid (analysis time of 5 min for etidronate and clodronate and 7 min for alendronate and pamidronate), and demonstrate precision (relative standard deviation was lower than 2.0% in all concentrations), accuracy, and specificity. Calibration curves are linear with r(2) > 0.99 over the concentration range of 50 to 400 microg/mL for etidronate and clodronate, and of 100 to 500 microg/mL for pamidronate and alendronate. Furthermore, they employed silica-based columns, which are cheaper than polymeric columns frequently used in previous reported methods.

Rapid analysis of alkylphosphonate drugs by capillary zone electrophoresis using indirect ultraviolet detection

“…Determination of CLO and ALN was performed by HPLC-MS [17,18] and HPLC with pre-or post-column derivatization using UV or fluorescent detectors [19][20][21][22][23][24][25]. Ion chromatography using different detection techniques was also employed for the analysis of CLO and ALN including indirect UV detection [26,27], light scattering [28], post-column derivatization and UV [29], conductivity [30], inductively coupled plasma MS [31,32] and refractive index detection [33]. Other proposed methods are spectrophotometry and stopped-flow spectrofluorometry with sequential injection techniques [34], GC [35], voltammetry [36], direct UV detection via complexation of metal ion [37] and anion exchange chromatography [38].…”

Ion-pair reversed phase liquid chromatography with ultraviolet detection for analysis of ultraviolet transparent cations

“…To overcome this limitation, some methods based on the conventional HPLC system have been developed to quantitate different anions and cations. Indirect UV detection was used to quantitate UV-transparent charged molecules [25,26] based on the addition of ionic chromophore in mobile phase. Mix-mode LC with CAD and HILIC with ELSD methods were reported on the separation and detection of multiple cations and anions in pharmaceutical formulations [18][19][20][21][22]27,28].…”

Umweltanalytik mit Ionenchromatografie: Status quo und Zukunftsperspektiven

“…B. HEDP (1-Hydroxyethan-1,1-diphosphonsäure) zählen nach den Aminopolycarbonsäuren zu den wichtigsten synthetischen Komplexbildnern, die in Wasch-und Reinigungsmitteln sowie als Kalkbildungsinhibitoren in Kühlwasserkreisläufen Anwendung finden. Die IC-Analyse in technischen Formulierungen, geschlossenen Wasserkreisläufen, hochbelasteten industriellen Abwässern und begleitend zu Laborstudien ist seit langem Standard (Weiß 1991;Fischer 1993a,b;Schmidt und Brauch 2005;Fernandes et al 2007). Nach wie vor existiert kein Verfahren, dessen Empfindlichkeit ausreichen würde, um Polyphosphonate in Umweltmedien direkt nachzuweisen.…”