Spectrophotometric and fluorimetric determination of diazepam, bromazepam and clonazepam in pharmaceutical and urine samples

• Published in: Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy Molecular and biomolecular spectroscopy, 2004-03, Vol.60 (4), p.771-780
• Main Authors: Salem, A.A, Barsoum, B.N, Izake, E.L
• Format: Article
• Language: English
• Subjects: Anti-Anxiety Agents - analysis; Anti-Anxiety Agents - urine; Anticonvulsants - analysis; Anticonvulsants - urine; Benzodiazepines; Biological samples; Bromazepam; Bromazepam - analysis; Bromazepam - urine; Calibration; Chromatography, High Pressure Liquid; Clonazepam; Clonazepam - analysis; Clonazepam - urine; Diazepam; Diazepam - analysis; Diazepam - urine; Humans; Hydroxides - chemistry; Light; Pharmaceutical preparations; Pharmaceutical Preparations - analysis; Potassium Compounds - chemistry; Spectrofluorimetry; Spectrometry, Fluorescence - methods; Spectrophotometry; Spectrophotometry - methods; Urine
• ISSN: 1386-1425
• DOI: 10.1016/S1386-1425(03)00300-7

New spectrophotometric and fluorimetric methods have been developed to determine diazepam, bromazepam and clonazepam (1,4-benzodiazepines) in pure forms, pharmaceutical preparations and biological fluid. The new methods are based on measuring absorption or emission spectra in methanolic potassium hydroxide solution. Fluorimetric methods have proved selective with low detection limits, whereas photometric methods showed relatively high detection limits. Successive applications of developed methods for drugs determination in pharmaceutical preparations and urine samples were performed. Photometric methods gave linear calibration graphs in the ranges of 2.85–28.5, 0.316–3.16, and 0.316–3.16 μg ml −1 with detection limits of 1.27, 0.08 and 0.13 μg ml −1 for diazepam, bromazepam and clonazepam, respectively. Corresponding average errors of 2.60, 5.26 and 3.93 and relative standard deviations (R.S.D.s) of 2.79, 2.12 and 2.83, respectively, were obtained. Fluorimetric methods gave linear calibration graphs in the ranges of 0.03–0.34, 0.03–0.32 and 0.03–0.38 μg ml −1 with detection limits of 7.13, 5.67 and 16.47 ng ml −1 for diazepam, bromazepam and clonazepam, respectively. Corresponding average errors of 0.29, 4.33 and 5.42 and R.S.D.s of 1.27, 1.96 and 1.14 were obtained, respectively. Statistical Students t-test and F-test have been used and satisfactory results were obtained.