title: Transmission FTIR derivative spectroscopy for estimation of furosemide in raw material and tablet dosage form.
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.
authors.affiliation: Laboratorio de Espectroscopia Molecular, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101-A, Venezuela.
authors.forename: Máximo
authors.initials: M
authors.lastname: Gallignani
authors.affiliation: Laboratorio de Espectroscopia Molecular, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101-A, Venezuela.
authors.forename: Rebeca A
authors.initials: RA
authors.lastname: Rondón
authors.affiliation: Departamento de Análisis y Control, Facultad de Farmacia y Bioanálisis, Universidad de Los Andes, Mérida 5101-A, Venezuela.
authors.forename: José F
authors.initials: JF
authors.lastname: Ovalles
authors.affiliation: Laboratorio de Espectroscopia Molecular, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101-A, Venezuela.
authors.forename: María R
authors.initials: MR
authors.lastname: Brunetto
keywords: API, active pharmaceutical ingredient; DMF, N,N-dimethylformamide; DS, derivative spectroscopy; Derivative spectroscopy; FTIR; FTIR, Fourier transform infrared; FUR, furosemide or frusemide; Frusemide; Furosemide; HPLC, high performance liquid chromatographic; MIR, mid infrared; Pharmaceutical analysis