title: Application of the extraction induced by emulsion breaking for the determination of chromium and manganese in edible oils by electrothermal atomic absorption spectrometry.
abstract: This work reports the optimization of a method, based on the extraction induced by emulsion breaking, for the determination of trace concentrations of Cr and Mn in edible oils by electrothermal atomic absorption spectrometry (ETAAS). In the method, a water-in-oil emulsion was prepared by mixing the oil sample with an acid solution (HNO(3)) of Triton X-114 to allow the intense contact between the sample and the extractant acid solution. Afterwards, the emulsion was broken by heating and the acid aqueous phase deposited in the bottom of the flask was collected for the determination of the metals of interest. The method was optimized by studying the influence of several parameters such as the concentration of HNO(3) and the emulsifier agent (Triton X-100 and Triton X-114) in the extractant solution. The best results were verified when the procedure was performed with 5 mL of the sample and 1 mL of the extractant solution containing 15%m/v of Triton X-114 and 2.8 mol L(-1) of HNO(3). Also, the fastest emulsion breaking was verified when the emulsions were heated at 90°C. In these conditions, the emulsions were broken in approximately 10 min. The quantification of Cr and Mn in the extracts was carried out by external calibration with aqueous standard solutions, which simplified the procedure. The limits of detection for the determination of Cr and Mn in the oil samples were 66 and 36 ng L(-1), respectively, and the limits of quantification were 219 and 120 ng L(-1), respectively. The developed method was applied in the determination of Cr and Mn in twelve samples of edible oils produced with different oleaginous. Recovery tests were performed to attest the accuracy of the method, being observed recovery percentages in the range of 86-115%.
authors.affiliation: Departamento de Química Analítica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niterói/RJ, 24020-141, Brazil.
authors.forename: Nicolle F
authors.initials: NF
authors.lastname: Robaina
authors.forename: Daniel M
authors.initials: DM
authors.lastname: Brum
authors.forename: Ricardo J
authors.initials: RJ
authors.lastname: Cassella
mesh_terms: D002138:Calibration; D005591:Chemical Fractionation / Q000379:methods*; D002857:Chromium / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D045703:Emulsifying Agents / Q000737:chemistry; D004655:Emulsions; D005504:Food Analysis; D008345:Manganese / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D017942:Nitric Acid / Q000032:analysis; D009821:Oils / Q000737:chemistry*; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013696:Temperature; D013997:Time Factors; D014867:Water / Q000737:chemistry
chemical_list: D045703:Emulsifying Agents; D004655:Emulsions; D009821:Oils; D014867:Water; D002857:Chromium; D017942:Nitric Acid; D008345:Manganese