Simultaneous extraction of tocotrienols and tocopherols from cereals using pressurized liquid extraction prior to LC determination

Tocopherols and tocotrienols have been simultaneously determined in food samples using a rapid and simple analytical method including pressurized liquid extraction (PLE) and LC with electrochemical detection. Separation was carried out on a Phenomenex Synergi 4 μm Hydro‐RP 80A column, using a solution of 2.5 mM acetic acid/sodium acetate in methanol/water (99:1, v/v) as mobile phase at a flow rate of 1.0 mL/min. Column temperature was maintained at 30°C. Detection was performed by coulometric detection at 500 mV except for (β+γ)‐tocotrienol, in wheat and rye samples, which was at +350 mV. A palm oil containing a relatively large amount of γ‐tocotrienol and lower concentrations of α‐ and δ‐tocotrienols and α‐ and γ‐tocopherols was used to provide reference retention times for the tocotrienols. Analyte quantification was performed using the external standard method. The calibration equations of tocopherols were used to quantify both tocopherols and their corresponding tocotrienols. The extraction recoveries obtained using the optimized PLE conditions were in the 80–114% range, with RSDs lower than 15%. The method was successfully applied to the determination of tocotrienols and tocopherols in cereal (wheat, rye, barley, maize and oat) and palm oil samples.