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1 4 4 Vol. 4 No Journal of Food Safety and Quality Aug., 2013 * 赵电波, 张丽尧, 白艳红 (, ) 摘要 : 目的, (DBP) (DnOP) 方法 -, 0.45 μm, HP-5MS, GC-MS 结果, DBP DnOP, 200 PE, 60 min, DBP DnOP mg/kg;, DBP DnOP, h, DBP DnOP mg/kg, 4 48 h DBP DnOP mg/kg 4 DBP DnOP 25 结论 DBP DnOP, DBP DnOP 关键词 : ; ; ; ; Migration of dibutyl phthalate and di-n-octyl phthalate in food-grade plastic packaging bags applied in fried food packaging ZHAO Dian-Bo, ZHANG Li-Yao, BAI Yan-Hong * (College of Food and Biological Engineering, Zhengzhou University of Light Industry, Zhengzhou , China) ABSTRACT: Objective To investigate the migration of dibutyl phthalate (DBP) and di-n-octyl phthalate (DnOP) in food grade plastic packaging bag applied in fried bread stick packaging were investigated. Methods The samples were extracted with methanol- saturated n-hexane. The supernatant were separated by polar HP-5MS capillary column and analyzed by GC-MS after filtering through 0.45 μm membrane filter. Results The amount of migration of DBP and DnOP increased with the initial package temperature increasing. The amounts of migration of DBP and DnOP were 0.70 mg/kg and 0.16 mg/kg respectively in fritter samples which were packaged at 200 and then stored at room temperature for 60 min. The amount of migration of DBP and DnOP increased with the storage time prolonging after samples were packaged at 200 initial temperature. The amounts of migration of DBP and DnOP in fritter samples which were packaged at 200 and then stored at 25 for 48 h were 0.79 mg/kg and 0.24 mg/kg, respectively. The amounts of migration of DBP and DnOP in fritter samples which were packaged at 200 and then stored at 4 for 48 h were 0.63 mg/kg and 0.15 mg/kg, respectively. The amounts of migration of DBP and DnOP in the samples which were stored at 4 * 通讯作者 :,, baiyanhong@zzuli.edu.cn *Corresponding author: BAI Yan-Hong, Associate Professor, College of Food and Biological Engineering, Zhengzhou University of Light Industry, No.5, Dongfeng Road, Zhengzhou , China. baiyanhong@zzuli.edu.cn

2 were lower than that at 25. Conclusion The maximum amounts of migration of DBP and DnOP occurred in the skin of fritters which were directly contacted the packaging materials, and then migrated to the food inside. There was a potential hazard for the health of consumers because of the migration of DBP and DnOP. KEY WORDS: food grade plastic packaging bag; dibutyl phthalate; di-n-octyl phthalate; high temperature fried food; migration,, (phthalate esters, PAEs), (DBP) (DnOP) PAEs [1,2],,, [3-6], (USEPA) 6, DBP DnOP [7], Aurela [8] 29 ( ), 50% 5 mg/kg, DBP 200 mg/kg [9], DBP DnOP Saito [10] 29 11, 50%, DBP 0.09~0.19 mg/kg PAEs, PAEs, DBP DnOP 2.87 mg/kg 14.2 mg/kg [11] Petersen [12],, DBP DnOP,, DBP DnOP 1 材料与方法 1.1 材料与试剂 PE ; ( cm, ); ( ) : (DBP) (DnOP) Dr. Ehrenstorfer ; (, ); 1.2 仪器与设备 - (6890GC/5973MS, ); : HP-5MS (30 m 0.25 mm 0.25 μm); RE-52AA ( ); AL204 ( - ); XH-C ( ); UP2200HE ( ) 1.3 方法 标准溶液配制 : DBP DnOP 0.05 g, 50 ml, 1000 mg/l 2 1 ml,, 10 ml, 100 mg/l, 4, 色谱 / 质谱条件 : ; : 1.0 ml/min; : 4:1; : 1 μl; : 270 ; : 50, 20 /min 220, min; : 230 ; : 270 ; : EI; : ; : Amn

3 4, : 样品前处理方法 6 7,,,, PE,,, (2±0.1) g, 50 ml, 20 ml -,, min, 1 ml,, 1 ml,,, 0.45 μm, 1 μl, GC-MS 200, 2/3,, 1/3, DBP DnOP GC-MS, 包装初始接触温度对 DBP 和 DnOP 迁移量的影响, ,, (25 ) 60 min, DBP DnOP 包装接触时间对 DBP 和 DnOP 迁移量的影响, 200, (25 ) min,, DBP DnOP 储藏温度对 DBP 和 DnOP 迁移量的影响, 200, 25 4, h, DBP DnOP DBP 和 DnOP 在油条中的迁移性的研究 200, 2/3 PE, h,, DBP DnOP 2 结果与分析 2.1 标准溶液色谱图 HP-5MS(30 m) DBP DnOP, 1 20 min DBP DnOP,,,,, DBP DnOP DBP DnOP,, 1 DBP DnOP 0~100 mg/l, , 0.002~0.005 mg/l,, 1 μl, DBP DnOP DBP DnOP mg/kg, (2007/19/EC) [13] 1 DBP DnOP GC-MS Fig. 1 The GC-MS chromatogram of DBP and DnOP Table 1 表 1 GC-MS 法分析 DBP 和 DnOP 的回归方程 相关系数 线性范围和检出限 Regression equation, correlation coefficient, linear range and detection limit of DBP and DnOP by GC-MS 相关系数 (R 2 ) (mg/l) (mg/l) DBP Y=0.545X ~ DnOP Y=0.9196X ~

4 包装初始接触温度对 DBP 和 DnOP 迁移量的影响 DBP DnOP 2, DBP DnOP 100, DBP 0.39 mg/kg, (0.30 mg/kg) [13-16] 200,,, DBP 0.70 mg/kg, (0.30 mg/kg) [13-16] 200 DnOP 0.16 mg/kg [13,15,16] DnOP, SN/T DnOP 2.0 mg/kg [14], DnOP,,, PVC [17,18], DBP DnOP 2.3 包装接触时间对 DBP 和 DnOP 迁移量的影响 DBP DnOP 3 3, PE DBP DnOP, PE,, DBP DnOP 40 min, DBP 0.34 mg/kg, (0.30 mg/kg) [13-16] 40 min DBP 20 min 325.0% 60 min, DBP 0.70 mg/kg, [13-16] (0.30 mg/kg), DBP 40 min % 60 min, DnOP 0.16 mg/kg; DnOP 40 min 66.7% [13,15,16] DnOP, SN/T DnOP 2.0 mg/kg [14], DnOP,,, Goulas [19] Fugit [20] [21],, 2 DBP DnOP ( 60 min) Fig. 2 Effect of the initial package temperature on migration of DBP and DnOP (package time: 60 min) 3 DBP DnOP ( 200 ) Fig. 3 Effect of the package time on migration of DBP and DnOP (initial temperature: 200 )

5 4, : 包装后储藏温度对 DBP 和 DnOP 迁移量的影响 DBP DnOP 4 4, 25 4 DBP DnOP h, DBP [13-16] (0.30 mg/kg) ; h DBP (0.30 mg/kg) DnOP 0.24 mg/kg, [14] (2.0 mg/kg), DnOP 25, DBP DnOP 4 DBP DnOP (P 0.05), DBP DnOP 3 4, 1 min 60 min,, DBP DnOP, 1 h 48 h,, DBP DnOP 2.5 DBP 和 DnOP 在油条中的迁移行为 DBP DnOP PE 200, 25 1 h, DBP DnOP mg/kg, mg/kg; 4, DBP DnOP mg/kg, mg/kg DBP DnOP, 3 结论, DBP DnOP, DBP DnOP 200 PE 60 min, DBP DnOP mg/kg, DBP DnOP h, DBP DnOP mg/kg, 4 DBP DnOP 25 DBP DnOP 参考文献 4 DBP DnOP Fig. 4 Effect of the storage temperature on migration of DBP and DnOP [1] Xu XR, Li XY. Sorption behaviour of benzyl butyl phthalate on marine sediments: Equilibrium assessments, effects of organic carbon content, temperature and salinity [J]. Mar Chem, 2009, 115: [2] Bosnir J, Puntari D, Galic A, et al. Migration of phthalates from plastic containers into soft drinks and mineral water [J]. Food Technol Biotechnol, 2007, 45(1): [3] Kotowaka U, Garbowska K, Isidorov A. Distuibution coefficients of phthalates between absorption fiber and water and tis using in quantitative analysis [J]. Anal Chim Acta, 2006, 560: [4] Ito R, Miura N, Ushiro M, et al. Effect of gamma-ray irradiation on degradation of di(2-ethylhexyl) phthalate in polyvinyl chloride sheet [J]. Int J Pharm, 2009, 376: [5] Ishido M, Masuo Y, Sayato J. Dicyclohexyl phthalate causes hyperactivity in the rat Concomitantly with impairment of tyro-

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