Reagent-free determination of amikacin content in amikacin sulfate injections by FTIR derivative spectroscopy in a continuous flow system

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.

Application of 3A Zeolite Prepared from Venezuelan Kaolin for Removal of Pb (II) from Wastewater and Its Determination by Flame Atomic Absorption Spectrometry

This work consists in the use of a 3A zeolite (K-LTA) obtained by a process of exchange of sodium for potassium (4A zeolite), synthesized from Venezuelan kaolin for the removal of Pb (II) ions from aqueous solutions by batch process mode in order to consider its application in treating industrial wastewaters. The 3A zeolite was characterized for X-ray powder diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR) and scanning electron microscopy and energy dispersive X-ray microanalysis (SEM-EDX). The metal concentration in the equilibrium Ce (mg·L-1) after adsorption with 3A zeolite was analyzed using flame atomic absorption spectrometry (FAAS). The influences of the solution pH, contact time, metal initial concentration and adsorbent dosage have been studied. The retention of metal occurring at pH values around 6.5 and the adsorption equilibrium was obtained at 60 min. The equilibrium process was well described by Langmuir, Freundlich and Dubinin-Radushkevich (D-R) isotherm models. The Langmuir parameters qm (mg·g-1) and b (L·mg-1) (which are related to the sorption capacity and constant of sorption energy) obtained were 14.64 and 5.42 respectively. The Pb (II) experimental uptake was about 14.56 mg·g-1, a little smaller than the theoretical one given by Langmuir isotherm model. The regression parameters and correlation coefficients (R) indicate that the adsorption data for Pb (II) removal fit better the Langmuir isotherm model. Moreover, 0 1/n 1 (1/n is 0.13), indicating that adsorption of metal ions on the zeolite, is a favorable physical process. The application of removing of the metal lead from real samples was examined by industrial wastewater samples. For all samples, the percentage of recovery was found with accuracy of more than 98%. The present work suggests 3A zeolite used as a sorbent material with relatively low cost, obtained from Venezuelan raw material;it is a candidate for removal lead ion and probably other cationic heavy metal species from wastewater.

Transmission FTIR derivative spectroscopy for estimation of furosemide in raw material and tablet dosage form

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)(SO_(2) 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.