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On-line dilution flow injection manifold for the selective spectrophotometric determination of ascorbic acid based on the Fe(II)-2,2'-dipyridyl-2-pyridylhydrazone complex formation
Authors:Themelis D G  Tzanavaras P D  Kika F S
Institution:Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, 54006 Thessaloniki, Greece.
Abstract:A new simple and rapid FI method for the accurate and precise spectrophotometric determination of ascorbic acid (AsA) in pharmaceutical formulations is reported. The method is based on the reduction of Fe(III) to Fe(II) by the analyte, and the subsequent reaction of the produced Fe(II) with 2,2'-dipyridyl-2-pyridylhydrazone (DPPH) in acidic medium (pH ca. 2.5) to form a colored complex (lambda(max)=535 nm). An on-line dilution mode using a binary inlet static mixer (BISM) was incorporated in the FI system, allowing the determination of the analyte in a wide concentration range. The calibration graph was linear in the range of 5.7-600.0 mg l(-1) AsA, at a sampling rate of 120 injections h(-1). The method was found to be very precise s(r)=0.1% at 300 mg l(-1) AsA (n=12)] and the 3delta detection limit (c(L)=1.7 mg l(-1)) was quite satisfactory. The detailed study of various interferences confirmed the high selectivity of the proposed method. Its application to a variety of pharmaceuticals produced excellent results, with a mean relative error of e(r)<1.0%.
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