PMID- 12477186 OWN - NLM STAT- MEDLINE DCOM- 20030515 LR - 20190729 IS - 1060-3271 (Print) IS - 1060-3271 (Linking) VI - 85 IP - 6 DP - 2002 Nov-Dec TI - Sequential determination of salicylic and acetylsalicylic acids by amperometric multisite detection flow injection analysis. PG - 1253-9 AB - 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. FAU - Catarino, Rita I L AU - Catarino RI AD - University of Porto, CEQUP/Department of Physical Chemistry, Faculty of Pharmacy, Portugal. FAU - Garcia, M Beatriz Q AU - Garcia MB FAU - Lapa, Rui A S AU - Lapa RA FAU - Lima, Jose L F C AU - Lima JL FAU - Barrado, Enrique AU - Barrado E LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - J AOAC Int JT - Journal of AOAC International JID - 9215446 RN - 0 (Indicators and Reagents) RN - 0 (Solutions) RN - O414PZ4LPZ (Salicylic Acid) RN - R16CO5Y76E (Aspirin) SB - IM MH - Aspirin/*analysis MH - Chromatography, Gas MH - Chromatography, Liquid MH - Colorimetry MH - Electrochemistry MH - Electrodes MH - Flow Injection Analysis MH - Fluorometry MH - Indicators and Reagents MH - Portugal MH - Salicylic Acid/*analysis MH - Solutions MH - Spectrophotometry, Infrared MH - Spectrum Analysis, Raman EDAT- 2002/12/13 04:00 MHDA- 2003/05/16 05:00 CRDT- 2002/12/13 04:00 PHST- 2002/12/13 04:00 [pubmed] PHST- 2003/05/16 05:00 [medline] PHST- 2002/12/13 04:00 [entrez] PST - ppublish SO - J AOAC Int. 2002 Nov-Dec;85(6):1253-9.