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Article Abstracts

Published:Journal of Chromatographic Science, ISSN 0021-9665Volume 39, Number 10, October 2001, pp. 425-430

Quantitative Determination of the Loop Diuretic Bumetanide in Urine and Pharmaceuticals by High-Performance Liquid Chromatography with Amperometric Detection

M.J. Legorburu[1], R.M. Alonso[1], R.M. Jiménez[1], and E. Ortiz[2]
[1]Departamento de Química Analítica, Facultad de Ciencias, Universidad del País Vasco/EHU., Apdo. 644, 48080 Bilbao, Spain and [2]Departamento de Especialidades Médico-Quirúrgicas, Facultad de Medicina, Universidad del País Vasco/EHU., Apdo. 644, 48080 Bilbao, Spain

A high-performance liquid chromatographic method with amperometric detection has been developed for the determination of the diuretic bumetanide using a µBondapak C18 column. The mobile phase consists of a 50:50 acetonitrile–water mixture containing 5mM KH2PO4–K2HPO4 (pH 4.0). The compound is monitored at +1350 mV with an amperometric detector equipped with a glassy carbon working electrode. A liquid–liquid or solid–liquid extraction is done prior to chromatographic analysis in order to avoid the interferences found in the urine matrix. The percentages of recovery obtained are 71% ± 1% for liquid–liquid extraction and 84.2% ± 0.7% for solid–liquid extraction. The method developed has a linear concentration range from 50 to 499 ng/mL with a reproducibility in terms of relative standard deviation of 1.73% and 3.85% for a concentration level of 70 ng/mL and 237 ng/mL, respectively, and a detection limit of 0.25 ng/mL (3:1 signal-to-noise ratio). The method is applied to the determination of bumetanide in pharmaceutical formulations and urine obtained from hypertensive patients and healthy volunteers after the ingestion of a therapeutic dose of Fordiuran (1 mg bumetanide).

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