Screening for mineral oil hydrocarbons in vegetable oils by silver ion-planar solid phase extraction

Abstract

The analysis of mineral oil hydrocarbons in vegetable oils is challenging especially regarding the analysis of mineral oil aromatic hydrocarbons (MOAH) since native terpenes like squalene or β-carotene are usually extracted along with the MOAH fraction and interfere their detection. When applying a recently developed screening method for the analysis of mineral oil saturated hydrocarbons (MOSH) and MOAH in paper and cardboard by planar solid phase extraction (pSPE) to vegetable oils, native terpenes expectably interfered with MOAH analysis. Thus, an adaption of pSPE employing silver ions, named silver ion-planar solid phase extraction (Ag-pSPE), was developed in this study. Impregnation of thin-layers with silver nitrate (AgNO₃) was found to be very successful in retaining squalene and β-carotene. MOAH analysis of vegetable oils after saponification showed good repeatability (relative standard deviation (%RSD) <10%) and recoveries of 73.4-112.4% at a spiking level of 4.5 mg/kg (n = 4). For MOSH analysis, a simple solid phase extraction (SPE) clean-up with aluminum oxide removed native n-alkanes prior to Ag-pSPE. Recoveries for MOSH were 55.3-84.5% with %RSD <11% at a spiking level of 45.5 mg/kg (n = 4). Limits of decision and quantitation were at 7.2 and 22.2 ng/zone for MOSH and 1.1 and 3.4 ng/zone for MOAH, respectively, which corresponded to the recently introduced pSPE method, thus showing that analytes were not affected by the impregnation of HPTLC plates with AgNO₃. The method comparison with LC-GC showed similar results for MOSH, while the amounts for MOAH determined by Ag-pSPE were higher.

Keywords: High-performance thin-layer chromatography (HPTLC); Mineral oil saturated and aromatic hydrocarbons (MOSH and MOAH); Screening; Silver ion–planar solid phase extraction (Ag–pSPE); Ultraviolet and fluorescence detection (UV/FLD); Vegetable oils.