Issue 12, 2011

PARAFAC based methods for the analysis of Diltiazemdrug excitation emission matrices of fluorescence obtained by a derivatization reaction

Abstract

A fluorescent derivatization reaction for Diltiazem drug quantification based on the condensation reaction of citric or malonic acid with acetic anhydride, catalyzed by the tertiary amine group of Diltiazem, was developed. Excitation emission matrices (EEMs) of fluorescence of the pure solvent (ethanol), standard and sample solutions following a standard addition methodology were analysed by PARAFAC based methods (PARAFAC, PARAFAC2 and PARALIND) to obtain robust calibration methodologies. The quantification results of the sample were compared with the official US Pharmacopeia high performance liquid chromatography-ultraviolet method (USP HPLC-UV). Although the experimental sets of EEM show linearity deviations all the PARAFAC based methods allow correct robust estimation of Diltiazem concentration in pharmaceutical formulations. The closest results were: derivatization with citric acid and PARAFAC2 six components non-negativity constraint model with a detection limit of 0.088 ppm; and, derivatization with malonic acid and PARAFAC six components non-negativity constraint model with a detection limit of 0.066 ppm for the malonic acid was observed. The simultaneous utilization of the three PARAFAC methods gives further information about the intrinsic structure of the data sets under analysis, i.e., it works as an efficient diagnostic tool for the existence of non-linearity and colinearity.

Graphical abstract: PARAFAC based methods for the analysis of Diltiazem drug excitation emission matrices of fluorescence obtained by a derivatization reaction

Article information

Article type
Paper
Submitted
05 Sep 2011
Accepted
05 Oct 2011
First published
17 Nov 2011

Anal. Methods, 2011,3, 2758-2769

PARAFAC based methods for the analysis of Diltiazem drug excitation emission matrices of fluorescence obtained by a derivatization reaction

J. M. M. Leitão, E. F. C. Simões and J. C. G. Esteves da Silva, Anal. Methods, 2011, 3, 2758 DOI: 10.1039/C1AY05560G

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