1.Reagent-free determination of amikacin content in amikacin sulfate injections by FTIR derivative spectroscopy in a continuous flow system
Ovalles F. José ; Gallignani Máximo ; Brunetto R. María ; Rondón A. Rebeca ; Ayala Carlos
Journal of Pharmaceutical Analysis 2014;(2):125-131
The quantitative estimation of amikacin (AMK) in AMK sulfate injection samples is reported using FTIR-derivative spectrometric method in a continuous flow system. Fourier transform of mid-IR spectra were recorded without any sample pretreatment. A good linear calibration (r40.999, %RSDo 2.0) in the range of 7.7-77.0 mg/mL was found. The results showed a good correlation with the manufacturer's and overall they all fell within acceptable limits of most pharmacopoeial monographs on AMK sulfate.
2.Transmission FTIR derivative spectroscopy for estimation of furosemide in raw material and tablet dosage form.
Máximo GALLIGNANI ; Rebeca A RONDÓN ; José F OVALLES ; María R BRUNETTO
Acta Pharmaceutica Sinica B 2014;4(5):376-383
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.