Abstract
A novel home-made hybrid detection system was designed for simultaneous determination of caffeine (CAF), dipyrone (DIP) and ergotamine (ERG) in pharmaceutical preparations. Thus, ERG was determined by a fluorimetric signal and PLS-1 method for resolving DIP and CAF UV-Vis spectral data was used. The calibration curve for ERG was linear over the range 2.5-10 mg L-1. The calibration set consisted of 18 mixtures with 0.5 to 4 mg L-1 for CAF, 5 to 20 mg L-1 for DIP and 2.5 and 10 mg L-1 for ERG. Sample preparation prior to analysis was not required. A recovery study with the real samples was carried out and the obtained results were highly satisfactory.
Highlights
Ergotamine tartrate [(5S’)-12’hydroxy-2’-methyl3’,6’,18-trioxo-5-benzyl ergotaman (2R, 3R)-tartrate], (ERG); dipyrone [disodium salt of [(2,3-dihydro-1,5dimethyl-3-oxo-2-phenyl-1H-pyrazol-4-yl] methylamino) methanesulfonic acid], (DIP) and caffeine [1,3,7trimethylxanthine], (CAF) are usually joined in some pharmaceutical preparations and in several formulations
Chromatographic techniques are widely applied for determining these analytes in pharmaceutical preparations, but these methods present the disadvantages of relative high cost, time consumption and use large volumes of toxic organic solvents.[1, 2]
The simultaneous determination of ERG, DIP and CAF was not found in the literature
Summary
Ergotamine tartrate [(5S’)-12’hydroxy-2’-methyl3’,6’,18-trioxo-5-benzyl ergotaman (2R, 3R)-tartrate], (ERG); dipyrone [disodium salt of [(2,3-dihydro-1,5dimethyl-3-oxo-2-phenyl-1H-pyrazol-4-yl] methylamino) methanesulfonic acid], (DIP) and caffeine [1,3,7trimethylxanthine], (CAF) are usually joined in some pharmaceutical preparations and in several formulations. Chromatographic techniques are widely applied for determining these analytes in pharmaceutical preparations, but these methods present the disadvantages of relative high cost, time consumption and use large volumes of toxic organic solvents.[1, 2]. Methodologies such as FIA and SIA with spectrometric, fluorimetric and biamperometric detection has been reported for this purpose.[3,4,5,6,7,8,9] the simultaneous determination of ERG, DIP and CAF was not found in the literature. The application of chemometric techniques as PCR (Principal component regression), PLS1 and PLS2 (Partial least squares) to spectrophotometric and fluorimetric data are being used for the analysis of complex mixtures.[10,11,12,13,14,15,16] In this paper a new analytical method with home-made hybrid detection system for simultaneous determination of CAF, DIP and ERG in pharmaceutical preparations is proposed
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