7 10 Vol. 7 No. 10 2016 10 Journal of Food Safety and Quality Oct., 2016 王 * 颖, 刘海韵, 张桂芳, 王志昱, 张晓瑜, 孙兆鹏 (, 264003) 摘要 : 目的 方法 GB/T 21911-2008, : (1:1, V:V),, 结果,, (2- ) (DEHP)70% (DBP)60% (DIBP)45% (DINP)20%, DEHP 35.7%, DBP 58.3% 结论, 关键词 : ; - ; ; Determination of plasticizers in finished and bulk oil in Yantai WANG Ying, LIU Hai-Yun, ZHANG Gui-Fang, WANG Zhi-Yu, ZHANG Xiao-Yu, SUN Zhao-Peng * (Yantai Center for Disease Control and Prevention, Yantai 264003, China) ABSTRACT: Objective To investigate the migration of plasticizers from plastic packaging into finished and bulk oil in Yantai. Methods According to GB/T 21911-2008, the samples were extracted with ethyl acetate: cyclohexane (1:1, V:V), and purified with gel permeation chromatography. Gas chromatography-tandem mass spectrometry (GC-MS/MS) was used for qualitative and quantitative analysis. Results There were low detection rates of plasticizers in finished oils, but high rates in bulk oils. The detection rates of bis(2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP), diisobutyl phthalate (DIBP) and diisononyl phthalate (DINP) were 70%, 60%, 45% and 20%, respectively, and the exceeding rates of DEHP and DBP were respectively 35.7% and 58.3%. Conclusion The finished oil should be chosen when shopping, and bulk oil should not be stored in the non-food-grade plastic bucket as far as possible. KEY WORDS: plasticizers; gas chromatography-tandem mass spectrometry; finished and bulk oil; plastic packaging 1 引言 (phthalate acid esters, PAEs),, [1],, (DBP) (2- ) (DEHP) (DINP) [2],,, 基金项目 : (2013WS256) Fund: Supported by Science and Technology bureau of Yantai (2013WS256) * 通讯作者 :,, E-mail: 124731611@qq.com *Corresponding author: SUN Zhao-Peng, Supervisor Technician, Yantai Center for Disease Control and Prevention, Yantai 264003, China. E-mail: 124731611@qq.com
4268 7 [3.4] PAEs, PAEs,,, PAEs, [5],,, [6], (DMP) (DEP) (DIBP) (DBP) (DPP) (2- ) (DEHP) (DBEP) (DNOP) (DINP) 16,, 2 材料与方法 2.1 仪器与试剂 Schambeck SFD9414 ( ), Agilent7890-7000A ( ), N-EVAP112 ( Organomation ), QL-901 ( SI ) ( ) 16, 1000 mg/l 2.2 试验方法 2.2.1 溶液配制 0.5 1.0 2.0 4.0 8.0 mg/l 1: 1(V:V) 2.2.2 样品前处理 1, 15, 20, 2013 2 GB/T 21911-2008 [7], 0.5g, : (1: 1, V:V) 10 ml, 2 min, 0.45 μm 3, : (1: 1, V:V), 4.7 ml/min, 5.5~16.5 min, 2.0 ml, - (GC-MS/MS) 2.2.3 气相色谱 - 串联质谱条件 (1) HP-5MS, : 60, 1 min; 20 /min 220, 1 min; 5 /min 280, 4 min 250 (2) EI, 250, 280, (SIM), 70 ev, 5 min 1 3 结果与分析 16 1( 1), QQQ 2 2,, 26.7%; ;, DEHP 70%, DBP 60%, DIBP 45% DINP 20%, 95% 2011 551 : (2- ) (DEHP) (DINP) (DBP) 1.5 mg/kg 9.0 mg/kg 0.3 mg/kg, ; DEHP 35.7%, DBP 58.3%, 45%,, DEHP DBP [8], 4 结论, 10 ml,,, :, 3, 1 h, 200 2 h,,,,,,,
10, : 4269 表 1 Table 1 邻苯二甲酸酯类化合物质谱条件参数 MS parameters of phthalate acid esters (min) (ev) 1 DMP 7.812 163 77, 135, 194 wind 20 2 DEP 10.123 149 177, 121, 222 wind 25 3 DIBP 10.895 149 223, 205, 167 wind 25 4 DBP 11.086 149 223, 205, 121 wind 20 5 DMEP 11.903 59 149, 193, 251 wind 30 6 BMPP 12.225 149 251, 167, 121 wind 30 7 DEEP 12.673 45 72, 149, 221 wind 25 8 DPP 14.784 149 237, 219, 167 wind 25 9 DHXP 14.925 104 149, 76, 251 wind 20 10 BBP 16.234 149 91, 206, 238 wind 25 11 DBEP 16.901 149 223, 205, 278 wind 30 12 DCHP 17.077 149 167, 83, 249 wind 15 13 DEHP 19.482 149 167, 279, 113 wind 25 14 DPHP 20.118 225 77, 153, 197 wind 25 15 DNOP 20.586 149 279, 167, 261 wind 20 16 DINP 20.865 57 149, 71, 167 wind 25 Fig. 1 1 16 Total ion chromatogram of 16 kinds of plasticizers standards
4270 7 Table 2 表 2 成品及散装食用油中塑化剂的检测结果 Detection results of plasticizers in finished and bulk oil DIBP DBP DPP DEHP DMP DEP DMEP BMPP DEEP DHXP BBP DBEP DCHP DPHP DNOP DINP 1 <0.05 <0.05 <0.05 0.078 <0.05 <0.10 2 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 3 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 4 <0.05 <0.05 <0.05 0.16 <0.05 <0.10 5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 6 <0.05 <0.05 <0.05 <0.05 <0.05 0.22 7 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 8 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 9 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 10 <0.05 0.42 <0.05 <0.05 <0.05 <0.10 11 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 12 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 13 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 14 0.13 0.15 <0.05 <0.05 <0.05 <0.10 15 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 6.7% 13.3% 0% 13.3% 0 6.7% 16 <0.05 <0.05 <0.05 1.15 <0.05 2.52 17 0.087 0.089 <0.05 0.85 <0.05 <0.10 18 <0.05 0.15 <0.05 1.21 <0.05 <0.10 19 <0.05 0.39 <0.05 1.74 <0.05 <0.10 20 <0.05 0.64 <0.05 0.45 <0.05 <0.10 21 0.24 0.35 <0.05 <0.05 <0.05 3.24 22 <0.05 0.23 <0.05 1.01 <0.05 <0.10 23 0.14 <0.05 <0.05 <0.05 <0.05 <0.10 24 <0.05 <0.05 <0.05 <0.05 <0.05 <0.10 25 0.96 0.36 <0.05 1.61 <0.05 <0.10 26 <0.05 <0.05 <0.05 1.85 <0.05 <0.10 27 <0.05 <0.05 <0.05 2.05 <0.05 4.02 28 <0.05 <0.05 <0.05 1.14 <0.05 <0.10 29 0.54 <0.05 <0.05 1.09 <0.05 <0.10 30 <0.05 <0.05 <0.05 0.96 <0.05 1.27 31 0.11 0.79 <0.05 <0.05 <0.05 <0.10 32 0.89 0.86 <0.05 1.75 <0.05 <0.10 33 <0.05 0.43 <0.05 1.83 <0.05 <0.10 34 0.36 0.28 <0.05 <0.05 <0.05 <0.10 35 0.45 0.14 <0.05 <0.05 <0.05 <0.10 45% 60% 0% 70% 0% 20%
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