Abstract

The application of multivariate calibration techniques to multicomponent analysis by UV-VIS molecular absorption spectrometry is a powerful tool for simul- taneous determination of several chemical species. However, when this methodol- ogy is accomplished manually, it is slow and laborious, consumes high amounts of reagents and samples, is susceptible to contaminations and presents a high opera- tional cost. To overcome these drawbacks, a flow-batch analyser is proposed in this work. This analyser was developed for automatic preparation of standard calibration and test (or validation) mixtures. It was applied to the simultaneous determination of Cu 2+ , Mn 2+ and Zn 2+ in polyvitaminic and polymineral pharmaceutical formula- tions, using 4-(2-piridilazo) resorcinol as reagent and a UV-VIS spectrophotometer with a photodiode array detector. The results obtained with the proposed system are in good agreement with those obtained by flame atomic absorption spectrometry, which was employed as reference method. With the proposed analyser, the prepara- tion of calibration and test mixtures can be accomplished about four hours, while the manual procedure requires at least two days. Moreover, it consumes smaller amounts of reagents and samples than the manual procedure. After the preparation of calibration and test mixtures, 60 samples h -1 can be carried out with the proposed flow-batch analyser.

Highlights

  • Nowadays, several techniques for simultaneous determination of chemical species exist, such as X-Ray Fluorescence Spectrometry (XRFS) [1, 2], Atomic and Molecular Fluorescence Spectrometry (AFS and MFS) [3, 4], Chromatography [5], Atomic Emission Spectrometry (AES), among others [6]

  • To compare the results obtained by flow-batch approaches (FBA)-SMA with those obtained by the flame atomic absorption spectrometry (FAAS) method, it was assumed that the determined metals were present in the samples as sulphates (MSO4.nH2O), which is more stable [41] according to the vademecum of the drugs

  • As well as other flow-batch systems, the FBA-SMA presents the advantage of the flexibility in the preparation of the calibration and test mixtures

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Summary

Introduction

Several techniques for simultaneous determination of chemical species exist, such as X-Ray Fluorescence Spectrometry (XRFS) [1, 2], Atomic and Molecular Fluorescence Spectrometry (AFS and MFS) [3, 4], Chromatography [5], Atomic Emission Spectrometry (AES), among others [6]. The UV-VIS Molecular Absorption Spectrometry (UV-VIS-MAS) [7] is an analytical method broadly used, due to its simplicity and fast achievement of experimental results. It is classically accomplished, by using chromogenic reagents. A specific reagent for each analyte can be used

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