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Sequential determination of salicylic and acetylsalicylic acids by amperometric multisite detection flow injection analysis.

Title
Sequential determination of salicylic and acetylsalicylic acids by amperometric multisite detection flow injection analysis.
Type
Article in International Scientific Journal
Year
2002
Authors
Catarino RI
(Author)
Other
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Garcia MB
(Author)
Other
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Barrado E
(Author)
Other
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Journal
Vol. 85 No. 6
Pages: 1253-1259
ISSN: 1060-3271
Publisher: AOAC INTERNATIONAL
Indexing
Scientific classification
FOS: Medical and Health sciences > Other medical sciences
CORDIS: Health sciences
Other information
Authenticus ID: P-000-MHT
Resumo (PT): An amperometric multisite detection flow injection analysis (FIA) system was developed for sequential determination of 2 analytes with a single sample injection and single detector. Tubular composite carbon electrodes with an inner diameter similar to that of the FIA manifold tubing were constructed so that measurements could be made without impairing the sample plug hydrodynamic characteristics. The electrochemical behavior of the tubular voltammetric cell in a low-dispersion FIA manifold and the behavior of the FIA system incorporating this type of voltammetric cell intended for multisite detection were evaluated by performing measurements with potassium hexacyanoferrate(II). Feasibility of the approach was demonstrated in the sequential determination of salicylic and acetylsalicylic acids in pharmaceutical products at a fixed potential of 0.98 V. The system allows sequential determination of salicylic acid concentrations ranging from 1.0 x 10(-5) to 5.0 x 10(-5) M and acetylsalicylic acid concentrations between 1.0 x 10(-3) and 5.0 x 10(-3) M with good precision on both detection sites and with relative standard deviations (RSDs) > or = 1.5% (n = 10) and 2.1% (n = 10), respectively. A comparison of these results with those of the U.S. Pharmacopeia procedure showed RSDs <5.0 and 1.0% for salicylic acid and acetylsalicylic acid, respectively. The proposed method enables 15 determinations per hour, which corresponds to the analysis of approximately 8 samples per hour. The detection limits of the methodology were approximately 3.5 x 10(-6) and 1.1 x 10(-5) M, respectively, for the first and second monitoring sites. <br> <br>
Abstract (EN): An amperometric multisite detection flow injection analysis (FIA) system was developed for sequential determination of 2 analytes with a single sample injection and single detector. Tubular composite carbon electrodes with an inner diameter similar to that of the FIA manifold tubing were constructed so that measurements could be made without impairing the sample plug hydrodynamic characteristics. The electrochemical behavior of the tubular voltammetric cell in a low-dispersion FIA manifold and the behavior of the FIA system incorporating this type of voltammetric cell intended for multisite detection were evaluated by performing measurements with potassium hexacyanoferrate(II). Feasibility of the approach was demonstrated in the sequential determination of salicylic and acetylsalicylic acids in pharmaceutical products at a fixed potential of 0.98 V. The system allows sequential determination of salicylic acid concentrations ranging from 1.0 x 10(-5) to 5.0 x 10(-5) M and acetylsalicylic acid concentrations between 1.0 x 10(-3) and 5.0 x 10(-3) M with good precision on both detection sites and with relative standard deviations (RSDs) > or = 1.5% (n = 10) and 2.1% (n = 10), respectively. A comparison of these results with those of the U.S. Pharmacopeia procedure showed RSDs <5.0 and 1.0% for salicylic acid and acetylsalicylic acid, respectively. The proposed method enables 15 determinations per hour, which corresponds to the analysis of approximately 8 samples per hour. The detection limits of the methodology were approximately 3.5 x 10(-6) and 1.1 x 10(-5) M, respectively, for the first and second monitoring sites. <br> <br>
Language: English
Type (Professor's evaluation): Scientific
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