Citation: KE Run-Hui, YANG Chun-Yan, HU Xue, XIE Rui-Long, YIN Jian-Jun, SONG Quan-Hou. Off-line Solid Phase Extraction Combined with Gas Chromatography-Flame Ionization Detection Method for Determination of Mineral oil Saturated and Aromatic Hydrocarbons in Olive Oils[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(10): 1677-1684. doi: 10.11895/j.issn.0253-3820.171520 shu

Off-line Solid Phase Extraction Combined with Gas Chromatography-Flame Ionization Detection Method for Determination of Mineral oil Saturated and Aromatic Hydrocarbons in Olive Oils

1.
China National Research Institute of Food & Fermentation Industries, National Food Quality Supervision and Inspection Center, Beijing 100015, China;
2.
Inner Mongolia Yili Industrial Group Co., Ltd., Hohhot 010080, China

Received Date: 18 December 2017
Revised Date: 6 August 2018

A method for quantitative analysis of mineral oil saturated hydrocarbons (MOSH) and aromatic hydrocarbons (MOAH) in olive oils by solid phase extraction (SPE) combined with programmed temperature vaporizer-gas chromatography-flame ionization detection (PTV-GC-FID) was established. The samples were dissolved in hexane, purified by the means of epoxidation combined with self-made molecular sieve SPE column and 0.3% silver nitrate silica SPE column alternating purification mode, in which way the interfering substances of lipids, wax esters, olefins and natural alkenes were removed, and the MOSH and MOAH fractions were effectively separated. The fractions were then concentrated by nitrogen, analyzed by the GC with large volume injection, separated by the capillary columns of DB-1, determined by a flame ionization detector, and quantified by external standard method. In addition, the key experimental parameters were optimized, including the amount of epoxidation reagent (mCPBA), epoxidation reaction time and elution volume. Under the optimized experimental conditions, Gravex913 lubricating oil showed good linearity as a standard reference of mineral oil in the ranges of 2.0-500.0 mg/L, the limits of detection (LOD) of MOSH and MOAH fractions were 0.3 mg/kg and 1.0 mg/kg, the limits of quantification (LOQ) were 1.0 mg/kg and 3.0 mg/kg, respectively. The spiked recoveries of MOSH and MOAH fractions were in the range of 93.2%-103.7% and 78.5%-81.3% at three spiked levels with the relative standard deviations (RSDs) of 2.7%-5.0% and 2.9%-4.0% (n=6). The established method has many advantages such as good purification effect, low reagent consumption and low detection limit, and is suitable for the separation and quantification of MOSH and MOAH in olive oils.
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沈阳化工大学材料科学与工程学院沈阳 110142