| Institution: | aLaboratorio de Espectroscopia Molecular, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101-A, Venezuela;bDepartamento de Análisis y Control, Facultad de Farmacia y Bioanálisis, Universidad de Los Andes, Mérida 5101-A, Venezuela |
| Abstract: | A Fourier transform infrared derivative spectroscopy (FTIR-DS) method has been developed for determining furosemide (FUR) in pharmaceutical solid dosage form. The method involves the extraction of FUR from tablets with N,N-dimethylformamide by sonication and direct measurement in liquid phase mode using a reduced path length cell. In general, the spectra were measured in transmission mode and the equipment was configured to collect a spectrum at 4 cm−1 resolution and a 13 s collection time (10 scans co-added). The spectra were collected between 1400 cm−1 and 450 cm−1. Derivative spectroscopy was used for data processing and quantitative measurement using the peak area of the second order spectrum of the major spectral band found at 1165 cm−1 (SO2 stretching of FUR) with baseline correction. The method fulfilled most validation requirements in the 2 mg/mL and 20 mg/mL range, with a 0.9998 coefficient of determination obtained by simple calibration model, and a general coefficient of variation <2%. The mean recovery for the proposed assay method resulted within the (100±3)% over the 80%–120% range of the target concentration. The results agree with a pharmacopoeial method and, therefore, could be considered interchangeable.KEY WORDS: FTIR, Derivative spectroscopy, Furosemide, Frusemide, Pharmaceutical analysisAbbreviations: API, active pharmaceutical ingredient; DMF, N,N-dimethylformamide; DS, derivative spectroscopy; FTIR, Fourier transform infrared; FUR, furosemide or frusemide; HPLC, high performance liquid chromatographic; MIR, mid infrared |
