6 12 Vol. 6 No. 12 2015 12 Journal of Food Safety and Quality Dec., 2015 周雅静 *, 钱凯, 杨心洁, 寇海娟 (, 213022) 摘要 : 目的, 方法 / (GC-MS) ESBO 结果 13 (57 ) 5 6 ESBO ESBO (30 mg/kg), 55.3 mg/kg 52.3 mg/kg 结论, ESBO 关键词 : ; ; ; ; Migration analysis and screening of epoxidized soy bean oil in imported infant food ZHOU Ya-Jing *, QIAN Kai, YANG Xin-Jie, KOU Hai-Juan (Changzhou Safety Testing Center for Entry-Exit Industrial and Consumable Products, Changzhou 213022, China) ABSTRACT: Objective To establish a method suitable for the determination of depoxy soybean oil in food, and to screen imported baby food that contaminated by depoxy soybean oil. Methods Gas chromatography/ mass spectrometry (GC-MS) had been used for the migration determination and screening the quantitative ESBO in imported baby foods. Results Totally 13 different kinds of baby food (57 samples) from 5 countries of European Union were screened. As a result, the level of ESBO in 6 kinds of infant food exceeds the European children's food ESBO limitation, which was 30 mg/kg. Two top ESBO values were 55.3 mg/kg of vegetables duck meat and 52.3 mg/kg of pasta vegetables meat, respectively. Conclusion From the test and the results of the screening, the level of ESBO in the high fat content of the baby food is relatively high. KEY WORDS: imported infant food; epoxidized soybean oil; migration; contamination; screening 1 引言, (ESBO) ESBO,, (PVC) [1], PVC, [2], ESBO PVC,, ESBO,, PVC, 50%, * 通讯作者 :,, E-mail: cathryn_821208@163.com *Corresponding author: ZHOU Ya-Jing, Master, Changzhou Testing Center for Entry-Exit Industrial and Consumable Product, No.1268, Longjn Road, Xinbei District, Changzhou 213022, China. E-mail: cathryn_821208@163.com
5078 6,, PVC, 35% ESBO, [3], (SCF) ESBO, (TDI) 1 mg/kg [4] (Heath and Reilly 1982, EPA/OTS 1987), ( ) [5], ( ),, ESBO ESBO, ESBO [6], ESBO,, (ESBO), PVC, GB 9695-2008 [7],, 1999 (scientific committee for food, SCF) ESBO (TDI) 1 mg/kg, 2002/72/EC, TDI (SML) 60 mg/kg 2004~2008, (JRC), PVC, 500 mg/kg, ESBO 1150 mg/kg, TDI,, 2007, 372/2007/EC ESBO (SML), 60 mg/kg, 30 mg/kg [8-10], 2008 579/2008/EC 372/2007/EC 2009 4 30, ESBO [12], ESBO, 2 材料与方法 2.1 仪器设备 7890GC-5975 MSD, Agilent( ); AG 285 ; 12, ; (Stand Vortex Mixer), Henry Troemmer. LLC;, ;, ;, ;, ELGA 2.2 试剂, GB/T 6682 ESBO : Accustandard Inc, 99.7%; ( ): Fluka Analytical; ( ): ( ) ; ( ): ; ( ): ; ( ): Acros Orgaincs; ( ): Sigma Aldrich; ( ): ; ( ): ; ( ): : 0.02 g (2.2.3) 20 ml, 4.0 ml,,, 5 min,, (2 mol/l): 10.7 g ( 0.1 g) 100 ml,, (10.0 g/l): 1.0 g ( 0.1mg) 100 ml,
12, : 5079, 10.0 g/l : -20 8, 6 (2500 mg/l): 2.4 ml 10 ml,, 2500 mg/l : 99.99% 2.3 样品的选择和种类, 1 Table 1 表 1 筛查样品的种类和产地 The type and origin of screening samples 3 21 3 3 3 4 3 4 3 9 3 8 3 8 3 8 3 8 3 6 3 4 2.3 实验方法 2.3.1 检测原理,,, 1,3-,,,, MS 2.3.2 样品的前处理 0.1 g 15 ml, 4.0 ml, 1 min, 4000 r/min 3 min, 30 min 3.0 ml, 5.0 ml 2,2,4-, 0.5 ml 5 min, 8 ml 2 mol/l, 1 min, 5.0 ml 3, GC-MS 2.3.3 GC/MS 的分析方法 GC/MS 7890-5975 GC-MS EI (70 ev) HP-5: 325 : 30 m 320 μm 0.25 μm 1 ml/min 290 300, 140 ( 2 min), 20 /min 300 ( 10 min) 1 μl, 1:40 (SIM), m/z 309, m/z 277, 367, 396 2.3.4 婴儿食品中 ESBO 的萃取步骤, 30.0 g 2 100 ml / (1:1, V:V), 23, 30 min, 1,3-2.3.5 脂肪含量的测定方法, 2.3.6 ESBO 定量方法 ESBO GC-MS 99.9%
5080 6, ESBO GC-MS, (SIM) : ESBO m/z 277, 309 GC-MS, ESBO ESBO ESBO 2, 2, 3 结果与讨论 3.1 分析方法的定性 55%, 25%, 8%, 11% : (C18:2E), 1 ESBO, 4 5 (C18:2E)Me 1,3-2, 3 (C16:0)Me (C18:0)Me 4 1,3- (C18:2E) m/z 277 309 m/z 309 1 ESBO Fig. 1 Chromatogram of commercial ESBO obtained by application of the developed method. 1: (C16:0)Me; 2: (C18:0)Me; 3: (C18:1E)Me 1,3- ; 4/5: (C18:2E)Me 1,3- Peaks: 1. (C16:0)Me; 2.(C18:0)Me; 3. 1,3-dioxolane of (C18:1E)Me; 4/5. Stereoisomers of 1,3-dioxolane of (C18:2E)Me 2 (C16:0)Me Fig. 2 Mass spectrum of (C16:0)Me
12, : 5081 3 (C18:0)Me Fig. 3 Mass spectrum of (C18:0)Me 4 (C18:2E)Me Fig. 4 Mass spectrum of (C18:2E)Me 5 (C18:2E)Me 1,3- Fig. 5 Mass spectrum of stereoisomers of (C18:2E)Me
5082 6 3.2 ESBO 筛查结果 ESBO (mg/kg), 2 7 ESBO, 6 ESBO 30 mg/kg ESBO ESBO ESBO 55.3 mg/kg 52.3 mg/kg ESBO 表 2 不同的食品检测所得 ESBO 的浓度 Table 2 ESBO concentrations in different food species % ESBO (mg/kg) 0.2 * 0.4 * 0.8 28.0 0.1 * 2.3 42.3 0.3 * 2.6 55.3 0.3 * 2.5 40.9 0.3 * 2.5 32.0 2.5 52.3 2.5 39.4 * 5 mg/kg, ESBO <5 mg/kg 4 结论, / (GC-MS) ESBO, 13 (57 ) 5 6 ESBO ESBO (30 mg/kg), 55.3 mg/kg 52.3 mg/kg,, ESBO 参考文献 [1] Baltacioğlu H, Balkö D. Effect of zinc stearate and/or epoxidized soybean oil on gelation and thermal stability of PVC-DOP plastigels [J]. J Appl Polym Sci, 1999, 74: 2488 2498. [2] Shepherd MJ, Gilbert J. Studies on the stabilization of poly(vinyl chloride) with epoxides transformation products and their migration from packaging to foods [J]. Eur Polym J, 1981 17, 285 289. [3] Demertzis PG, Riganakos KA, Akrida-Demertzi K. Gas chromatographic studies on polymer-plasticizer com-patibility: interactions between food-grade PVC and epoxidized soybean oil [J]. Eur Polym J, 1991, 27: 231 235. [4] Hammarling L, Gustavsson H, Svensson K, et al, Migration of epoxidized soya bean oil from plasticized PVC gaskets into baby food [J]. Food Addit Contam, 1998, 15: 203 208. [5] Hammarling L, Survey of epoxidised soya bean oil (ESBO) migration from plasticised gaskets [J]. Food Addit Contam, 1998, 15(2): 203 208. [6] The European Commission EU 10/2011, Commission Regulation(EU) No 10/2011 of 14 January 2011 on plastic materials and articles intended to come into contact with food [S]. 2011. [7] GB 9685-2008 [S]. 2008. GB 9685-2008 Food containers and packaging materials additives health standards [S]. 2008. [8] Fantoni L, Simoneau C, European survey on the contamination of homogenised baby food by epoxidised soybean oil from plasticised PVC gaskets [J]. Food Addit Contam, 2003, 20: 1087 1096. [9] Fankhauser-Noti A, Fiselier K, Biedermann S, et al. Epoxidized soy bean oil (ESBO) migrating from the gaskets of lids into food packed in glass jars [J]. Eur Food Res Technol, 2005, 221: 416 422. [10] Castle L, Sharman M, Gilbert J. Gas chromatographic-mass spectrometric determination of expoxidized soybean oil contamination of foods by migration from plastic packaging [J]. Food Addit, 1988, 71(6): 1183 118 作者简介 ( 责任编辑 : 白洪健 ) 周雅静, 硕士, 工程师, 主要研究方向为食品接触材料的分析检测 E-mail: cathryn_821208@163.com