Abstract: An alternative method based on an off-line solid phase extraction (SPE) combined with gas chromatography-flame ionization detection (GC-FID) method was developed to determine mineral oil saturated hydrocarbons (MOSH) in Chocolate. The MOSH was extracted with n-hexane. The extract was purified by solid phase extraction (SPE) on a column packed with silica gel impregnated silver nitrate. By comparing the purification effect of silica gel with different silver nitrate content, 0.3% (w/w) silver nitrate silica gel was determined to be the best, and a glass syringe was used as the container for filling silver nitrate silica gel, and the volume of eluent was determined to be 10 mL. The pooled eluate was concentrated and then injected into the GC-FID system. The inject temperature was 275 ℃. The GC column was heated from 50 ℃ to 60 ℃ at 2.5 ℃/min, and then raised to 280 ℃ at 22 ℃/min,and then raised to 320 ℃(12 min) at 30 ℃/min. FID temperature was set at 350 ℃. The GC injection volume was 2 μL. The results showed that the calibration curve of paraffin oil was linear in the range of 1-80 mg/kg with a correlation coefficient of 0.999. The quantification limit (LOQ) of MOSH in chocolate was 0.5 mg/kg. The recoveries from spiked samples were between 90.0% and 99.2%, with the relative standard deviation (RSD) of 6.1%-9.9%. The accuracy, precision and sensitivity of the method are in line with the requirements of saturated hydrocarbon mineral oil detection, and can be used for monitoring the contamination of saturated hydrocarbon mineral oil in chocolate.
[1] World Health Organization.Evaluation of certain food additives[J].World Health Organization Technical Report Series,2012(974):1-183. [2] 李克亚, 王志伟,胡长鹰.食品及食品包装纸中矿物油的研究进展//“食品工业新技术与新进展” 学术研讨会暨 2014 年广东省食品学会年会论文集[C].广州:广东省食品学会,2014:81-85. LI K Y,WANG Z W,HU C Y.Research progress of mineral oil in food and food packaging paper//“New Technology and New Progress in Food Industry” Symposium and Proceedings of the 2014 Guangdong Food Association Annual Conference[C].Guangzhou:Guangdong Food Association,2014:81-85. [3] BIEDERMANN M,UEMATSU Y,GROB K.Mineral oil contents in paper and board recycled to paperboard for food packaging[J].Packaging Technology and Science,2011,24(2):61-73. [4] BIEDERMANN M,GROB K.How “white” was the mineral oil in the contaminated Ukrainian sunflower oils[J].European Journal of Lipid Science and Technology,2009,111(4):313-319. [5] BARP L,KORNAUTH C,WÜGER T,et al.Mineral oil in human tissues,Part I:Concentrations and molecular mass distributions[J].Food and Chemical Toxicology,2014,72:312-321. [6] GROB K.Update on recycled paperboard and its compliance for food contact[J].Journal Für Verbraucherschutz und Lebensmittelsicherheit,2014,9(3):213-219. [7] VOLLMER A,BIEDERMANN M,GRUNDBÖCK F,et al.Migration of mineral oil from printed paperboard into dry foods:survey of the German market[J].European Food Research and Technology,2011,232(1):175-182. [8] 武彦文, 王颖,李冰宁,等.定量分析食品中的矿物油污染物[J].食品安全质量检测学报,2015,6(6):2 145-2 150. WU Y W,WANG Y,LI B N,et al.Quantitative analysis of mineral oil hydrocarbons in food[J].Journal of Food Safety & Quality,2015,6(6):2 145-2 150. [9] MORET S,GROB K,CONTE L S.On-line high-performance liquid chromatography-solvent evaporation - high-performance liquid chromatography - capillary gas chromatography - flame ionisation detection for the analysis of mineral oil polyaromatic hydrocarbons in fatty foods[J].Journal of Chromatography A,1996,750(1-2):361-368. [10] BARP L,PURCARO G,MORET S,et al.A high-sample-throughput LC-GC method for mineral oil determination[J].Journal of Separation Science,2013,36(18):3 135-3 139. [11] PURCARO G,ZOCCALI M,TRANCHIDA P Q,et al.Comparison of two different multidimensional liquid-gas chromatography interfaces for determination of mineral oil saturated hydrocarbons in foodstuffs[J].Analytical and Bioanalytical Chemistry,2013,405(2-3):1 077-1 084. [12] MORET S,BARP L,GROB K,et al.Optimised off-line SPE-GC-FID method for the determination of mineral oil saturated hydrocarbons (MOSH) in vegetable oils[J].Food Chemistry,2011,129(4):1 898-1 903. [13] MORET S,BARP L,PURCARO G,et al.Rapid and sensitive solid phase extraction-large volume injection-gas chromatography for the analysis of mineral oil saturated and aromatic hydrocarbons in cardboard and dried foods[J].Journal of Chromatography A,2012,1 243:1-5. [14] FISELIER K,GRUNDBÖCK F,SCHÖN K,et al.Development of a manual method for the determination of mineral oil in foods and paperboard[J].Journal of Chromatography A,2013,1 271(1):192-200. [15] 安红梅, 柯润辉,刘秀,等.固相萃取结合气相色谱-火焰离子化检测器分析面包中饱和烃类矿物油[J].食品与发酵工业,2016,42(1):152-156. AN H M,KE R H,LIU X,et al.Research on the determination of mineral oil saturated hydrocarbons (MOSH) in bread by SPE-GC-FID[J].Food and Fermentation Industries,2016,42(1):152-156. [16] BIEDERMANN M,GROB K.On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil.Part 1:Method of analysis[J].Journal of Chromatography A,2012,1 255:56-75. [17] FIORINI D,FISELIER K,BIEDERMANN M,et al.Contamination of grape seed oil with mineral oil paraffins[J].Journal of Agricultural and Food Chemistry,2008,56(23):11 245-11 250. [18] WHO.Evaluation of certain food additives[R].Geneva:WHO,2002. [19] FAO/WHO.Summary of evaluations performed by the joint FAO/WHO expert committee on food additives[J]. Nutrition Reviews,2000,58(3):90. [20] 杨春艳, 柯润辉,安红梅,等.食品中烃类矿物油的污染情况及迁移研究进展[J].食品与发酵工业,2017,43(2):258-264. YANG C Y,KE R H,AN H M,et al.Research progress on contamination and migration of mineral oil hydrocarbons in food[J].Food and Fermentation Industries,2017,43(2):258-264.
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