Open Chemistry · 2013 · 10 citations · 20 references
Natural SciencesChemistryPharmaceutical AnalysisAnalytical ChemistrySpectroscopic AnalysisSpectroscopyInstrumental AnalysisSample PreparationAssay DeterminationMethod Detection LimitThroughput
Abstract In this work, a flow-injection spectrophotometric method for dipyrone determination in pharmaceutical formulations was developed. Dipyrone sample solutions were injected into a carrier stream of deionized water and the reaction was carried out in a solid-phase reactor (12 cm, 2.0 mm i.d.) packed with Cu3(PO4)2(s) entrapped in a matrix of polyester resin. The Cu(II) ions were released from the solid phase reactor by the formation of Cu(II)-(dipyrone)n complex. When the complex is released, it reacts with 0.02% m/v alizarin red S in deionized water to produce a Cu(VABO3)3 complex whose absorbance was monitored at 540 nm. The calibration graph was linear over the range 5.0×10−5–4.0×10−4 mol L−1 with a detection limit of 2.0×10−5 mol L−1 and relative standard deviation for 10 successive determinations of 1.5% (2.0×10−4 mol L−1 dipyrone solution). The calculated sample throughput was 60 h−1. The column was stable for at least 8 h of continuous use (500 injections) at 25°C. Pharmaceutical formulations were analyzed and the results from an official procedure measurement were compared with those from the proposed FIA method in order to validate the latter method.
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