Determination of Synthetic Phenolic Antioxidants in Cake by HPLC/DAD after Mixed Micelle–Mediated Cloud Point Extraction

Abstract

A mixed micelle-mediated cloud point extraction (MMCPE) system was developed for the extraction and preconcentration of four synthetic phenolic antioxidants (SPAs) (propyl gallate (PG), tert-butylhydroquinone (TBHQ), butylated hydroxyanisole (BHA) and octyl gallate (OG) ) in cake. The mixture of two kinds of non-ionic surfactants polyoxy ethrlene nonyl phinyl ether (NP-7) and polyoxy ethrlene nonyl phinyl ether (NP-9) was utilized as a suitable micellar medium for preconcentration and extraction of SPAs. The surfactant-rich phase was then analyzed by high performance liquid chromatography-diode array detection (HPLC–DAD). The effect of different parameters such as concentration of surfactants, proportion of NP-7 and NP-9, equilibration time and temperature on the cloud point extraction (CPE) was carefully optimized. Under the studied conditions, four SPAs were successfully separated within 12 min. The relative standard deviations (RSD, n=6) were 1.2–2.0% and the limits of detection (LOD) were 1.5 ng mL₋1 for PG, 3.6 ng mL-1 for TBHQ, 2.9 ng mL-1 for BHA, and 0.8 ng mL-1 for OG, respectively. Recoveries of the SPAs in spiked cake samples were in the range of 92% to 99%. The MMCPE method showed potential advantage for the preconcentration of the SPAs, with enrichment factor of 25. Moreover, the method is simple, has high sensitivity, consumes much less solvent, and has significant advantage in extraction efficiency compared to traditional CPE methods.