Zhipu Xuebao (Jul 2024)
Determination of Migration of Four Sebacic Acid Esters in Food Contact Materials and Products by Gas Chromatography-Mass Spectrometry
Abstract
A method of gas chromatography-mass spectrometry (GC-MS) was established to determine the migration of dibutyl sebacate, dioctyl sebacate, diisooctyl sebacate, decanedioic acid bis(2,2,6,6-tetramethyl-4-piperidinyl)ester in water-based, acidic and alcoholic food simulants, and olive oil and chemical alternative solvents. The 95% ethanol and isooctane chemical substitution solutions were directly analyzed by GC-MS. The olive oil samples were extracted with acetonitrile followed by QuEChERS purification, and then analyzed by GC-MS. Other simulants (water, 4% acetic acid, 10% ethanol, 20% ethanol, and 50% ethanol) were extracted with n-hexane and then determined by GC-MS. The results showed that the method is well performed under optimized conditions, with the correlation coefficient (r2) greater than 0.995. The limits of detection and the limits of quantitation of the four sebacic acid ester compounds in water, 4% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, 95% ethanol, isooctane, and olive oil simulants are 0.1-0.2 mg/kg, 0.3-0.5 mg/kg, respectively. Migration experiments on plastic samples were conducted, and spiking experiments at three concentration levels of 0.30, 2.0, 4.0 mg/kg in water, 4% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, 95% ethanol, and isooctane food simulants, and three concentration levels of 0.50, 2.0, 4.0 mg/kg in olive oil food simulants were carried out. The spiking recoveries range from 92.5% to 108%, and the relative standard deviations (RSDs) are 2.4%-8.8%. The method solves the problem that decanedioic acid bis(2,2,6,6-tetramethyl-4-piperidinyl)ester cannot be extracted into n-hexane in 4% acetic acid by adjusting pH value using ammonium hydroxide, the optimal pH range was determined by comparing the responses of four targets at different pH values. QuEChERS was firstly used for migration experiments of sebacic acid esters in food contact materials to solve the turbidity and partial oil precipitation of olive oil simulants in the concentration process after extraction. By optimizing the QuEChERS filling material, the interference of organic acids, fatty acids, sugar and other impurities on the targets were reduced, producing greater separation effect of the targets. The separation efficiency of four chromatographic columns with different polarity was compared, and the DB-17HT column was selected to detect the four sebacic acid esters simultaneously. Plastics such as polypropylene, polyethylene terephthalic acid terephthalate, polyvinyl chloride, composite membranes, paper cups, recycled PET and recycled PVC were collected and migration experiments were carried out, the migration of sebacic acid esters in these plastics materials was investigated. This method is highly sensitive, precise, and accurate, fully meeting the requirement for determining the migration of the sebacic acid esters in food contact materials and their products.
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