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A rapid Fourier transform near-infrared (FT-NIR) spectroscopic method was developed for quantitative determination of the peroxide values (PVs) of edible oils. The method is based on the stoichiometric reaction of triphenylphosphine (TPP) with hydroperoxides to produce triphenylphosphine oxide (TPPO). Calibration standards were prepared by adding randomized amounts of TPPO and TPP to peroxide-free high-erucic-acid rapeseed (HEAR) to produce a calibration matrix spanning the concentrations of TPPO and residual TPP in oils having PVs in the range 0-100 after complete reaction of the hydroperoxides with added TPP. A partial-least-squares (PLS) calibration model for predicting PV was developed by using the NIR spectral region from 4710 to 4540 cm-1, where TPP and TPPO both absorb. The resulting PLS calibration was linear, the cross-validation having a standard deviation (SD) of 1.36 PV over the analytical range. The method was validated by comparing the PLS-predicted PVs of oils spiked with tert-butyl hydroperoxide (TBHP) and those of naturally oxidized HEAR oils with the results obtained by using the American Oil Chemists’ Society (AOCS) iodometric procedure. The FT-NIR PV method correlated very well (SD = 1.20) with the reference AOCS method for TBHP-spiked oil samples. Similar results were obtained for naturally oxidized HEAR oil, with a standard deviation of the difference for reproducibility of ±1.11 PV for both methods. The analysis consists of adding about 0.04 mL TPP stock solution to 1 g oil, shaking, recording the spectrum, and using the PLS calibration to predict PV. Because of its simple and rapid stoichiometric reaction and its excellent correspondence to the iodometric method, the FT-NIR method provides a simple and alternative means of measuring PV. The FT-NIR method avoids the solvent and reagent disposal problems associated with the AOCS method and can be readily auto mated by appropriate programming of the FTIR spectrometer. Thus, it provides a simple and rapid analytical technique for determining PVs of fats and oils.

Stoichiometric Determination of Hydroperoxides in Oils by Fourier Transform Near-Infrared Spectroscopy