Abstract
This chapter discusses the role of 13C nuclear magnetic resonance (13C-NMR) spectroscopy to determine methyl linoleate hydroperoxides. 13C-NMR spectra are recorded in deuterated chloroform (CDCl3) with a Brucker NMR spectrometer at 75.469 MHz operating in the pulse mode with Fourier transform at 37° and proton noise decoupling. The deuterium signal from CDC13 is used for the field frequency lock. 13C-NMR signals are accumulated 300 to 500 times with a 10 μsec pulse width and a 3.0 second pulse repetition time using 16.384 data points. The dienol mixtures isolated by preparative thin layer chromatography (TLC) are analyzed by both 13C-NMR and gravimetric high-performance liquid chromatography (HPLC). The 13C-NMR procedure described in the chapter provides an alternate approach to HPLC for the quantitative analysis of positional and geometric isomers of linoleate hydroperoxides formed by autoxidation. This direct analytical technique has the additional powerful advantage of providing detailed structural information on any new lipid hydroperoxides under investigation. The effective use of this method to analyze the allylic hydroperoxides of methyl oleate and of linoleate in this study indicates that it should also be applicable to the allylic hydroperoxides from other similar substrates.
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