Validated spectrofluorimetric method for the determination of clonazepam in pharmaceutical preparations.
A simple, highly sensitive and validated spectrofluorimetric method was applied in the determination of clonazepam (CLZ). The method is based on reduction of the nitro group of clonazepam with zinc/CaCl2, and the product is then reacted with 2-cyanoacetamide (2-CNA) in the presence of ammonia (25%) yielding a highly fluorescent product. The produced fluorophore exhibits strong fluorescence intensity at ʎ(em) = 383 nm after excitation at ʎ(ex) = 333 nm. The method was rectilinear over a concentration range of 0.1-0.5 ng/mL with a limit of detection (LOD) of 0.0057 ng/mL and a limit of quantification (LOQ) of 0.017 ng/mL. The method was fully validated and successfully applied to the determination of CLZ in its tablets with a mean percentage recovery of 100.10 ± 0.75%. Method validation according to ICH Guidelines was evaluated. Statistical analysis of the results obtained using the proposed method was successfully compared with those obtained using a reference method, and there was no significance difference between the two methods in terms of accuracy and precision.
Department of Analytical Chemistry, University of Mansoura, Mansoura, Egypt.
Fawzia
F
Ibrahim
Department of Analytical Chemistry, University of Mansoura, Mansoura, Egypt.
Nahed
N
El-Enany
Department of Analytical Chemistry, University of Mansoura, Mansoura, Egypt.
Shereen
S
Shalan
Department of Analytical Chemistry, University of Mansoura, Mansoura, Egypt.
Rasha
R
Elsharawy
D002998:Clonazepam / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D013050:Spectrometry, Fluorescence
D004364:Pharmaceutical Preparations; D002998:Clonazepam
2-cyanoacetamide; clonazepam; pharmaceutical preparations; reduction; spectrofluorimetry