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Exploiting the oxidative coupling reaction of MBTH for indapamide determination
David S M Ribeiro1, João A V Prior, João L M Santos
1REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia da Universidade do Porto, Rua Aníbal Cunha no. 164, 4050-047 Porto, Portugal.
Talanta
|July 21, 2009
Summary
An automated flow system rapidly quantifies indapamide in pharmaceuticals using oxidative coupling with 3-methylbenzothiazolin-2-one hydrazone (MBTH) and cerium(IV). This method offers accurate drug analysis with a high determination rate and low detection limit.
Area of Science:
- Analytical Chemistry
- Spectrophotometry
- Flow Injection Analysis
Background:
- Oxidative coupling reactions involving 3-methylbenzothiazolin-2-one hydrazone (MBTH) and cerium(IV) are established for quantitative analysis.
- Previous studies show varying optimal wavelengths for monitoring reaction products, necessitating further investigation.
- Indapamide, an antihypertensive diuretic, requires reliable analytical methods for pharmaceutical quality control.
Purpose of the Study:
- To develop and optimize an automated multipumping flow system for the spectrophotometric determination of indapamide.
- To evaluate the influence of reagent addition sequence on reaction kinetics, stability, and spectral properties.
- To apply the developed method for the accurate quantification of indapamide in pharmaceutical formulations.
Main Methods:
- Development of an automated multipumping flow system for oxidative coupling reaction.
- Optimization of the flow system using Plackett-Burman and central cubic faces experimental designs.
- Spectrophotometric detection of indapamide-MBTH-Ce(IV) reaction products.
- Validation against a reference procedure for pharmaceutical analysis.
Main Results:
- The sequence of reagent addition significantly impacts reaction kinetics, chemical stability, and absorbance spectra.
- The optimized automated system achieved rapid quantification of indapamide (approx. 25 h⁻¹).
- The method demonstrated high accuracy, with relative deviation under 2.1% compared to the reference procedure.
- A low detection limit of approximately 1 mg L⁻¹ was achieved.
Conclusions:
- An automated flow system utilizing the oxidative coupling of indapamide with MBTH and Ce(IV) provides a rapid and accurate method for pharmaceutical analysis.
- Experimental design is crucial for optimizing multipumping flow systems and understanding reaction parameter dependencies.
- The developed methodology is suitable for routine quality control of indapamide in pharmaceutical formulations.
