Microsoft Word 王颖-二校

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1 7 10 Vol. 7 No 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 (, ) 摘要 : 目的方法 GB/T , : (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 , China) ABSTRACT: Objective To investigate the migration of plasticizers from plastic packaging into finished and bulk oil in Yantai. Methods According to GB/T , 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 :,, @qq.com *Corresponding author: SUN Zhao-Peng, Supervisor Technician, Yantai Center for Disease Control and Prevention, Yantai , China @qq.com

2 [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 ( ), Agilent A ( ), N-EVAP112 ( Organomation ), QL-901 ( SI ) ( ) 16, 1000 mg/l 2.2 试验方法溶液配制 mg/l 1: 1(V:V) 样品前处理 1, 15, 20, GB/T [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) 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% : (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, 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.

3 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 , 135, 194 wind 20 2 DEP , 121, 222 wind 25 3 DIBP , 205, 167 wind 25 4 DBP , 205, 121 wind 20 5 DMEP , 193, 251 wind 30 6 BMPP , 167, 121 wind 30 7 DEEP , 149, 221 wind 25 8 DPP , 219, 167 wind 25 9 DHXP , 76, 251 wind BBP , 206, 238 wind DBEP , 205, 278 wind DCHP , 83, 249 wind DEHP , 279, 113 wind DPHP , 153, 197 wind DNOP , 167, 261 wind DINP , 71, 167 wind 25 Fig Total ion chromatogram of 16 kinds of plasticizers standards

4 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 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 < <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < < <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < % 13.3% 0% 13.3% 0 6.7% 16 <0.05 <0.05 < < < <0.05 < < < <0.05 < < < <0.05 < < < <0.05 < <0.05 <0.05 < < < <0.05 < <0.05 <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 <0.05 <0.05 < < <0.05 < <0.05 <0.05 < <0.05 < <0.05 <0.05 < < <0.05 <0.05 < <0.05 < <0.05 < <0.05 < <0.05 <0.05 < < <0.05 <0.05 <0.05 < < <0.05 < < < <0.05 < <0.05 <0.05 <0.05 < <0.05 <0.05 <0.05 < % 60% 0% 70% 0% 20%

10, : 4271,,,, 95%, 45%,, ph [9-12],,,, 参考文献 [1] 玥,,, 16 GC-MS [J]., 2014, 19(2): 94 99. Chu Y, Liang DP, Sun MY, et al.

National food contamination and hazardous factors risk of 2013 [M]. Beijing: China Standard Publishing House, 2012. [3],. [M]. :, 2006. Li C, Huang YM. Food safety monitoring and warning system [M].

5 10, : 4271,,,, 95%, 45%,, ph [9-12],,,, 参考文献 [1] 玥,,, 16 GC-MS [J]., 2014, 19(2): Chu Y, Liang DP, Sun MY, et al. Determination of 16 phthalate acid esters in foods by gas chromatography-massspectrometry [J]. J Chin Cereals Oils Ass, 2014, 19(2): [2], [M]. :, Yang DJ, Li N. National food contamination and hazardous factors risk of 2013 [M]. Beijing: China Standard Publishing House, [3],. [M]. :, Li C, Huang YM. Food safety monitoring and warning system [M]. Beijing: Chemical Industry Press, [4]. [J]., 2011, 11(1): Liu F. Application of plasticizer and its harm [J]. Guangdong Chem Ind, 2011, 11(1): [5],,, 21 - [J]., 2011, 30(10): Wu HQ, Zhu ZX, Huang XL, et al Study on determination of 21 phthalate acid esters and their distribution in different types of foods by gas chromatography-mass spectrometry [J]. J Insrtum Anal, 2011, 30(10): [6],. [J]., 2013, 38(5): 1 2 Cao JC, Jin QZ. Progress in contamination pathways and analysis methods of plasticizer in edible oil [J]. China Oils Fats, 2013, 38(5): 1 2. [7] GB/T [S]. GB/T The determination of phthalates in food [S]. [8],,. [J]., 2006, 26(5): Zheng Z, He JJ, Shao LM. Statistic analysis on distribution of phthalic acid esters in plastic packages [J]. Chin Environ Sci, 2006, 26(5): [9]. [J]., 2004, 25(6): Yao WR. The research situation of phthalate esters in food contaminants [J]. Food Res Dev, 2004, 25(6): [10] Le HH, Carlson EM, Chua JP, et al. Bisphenol A is released from polycarbonate drinking bottles and mimics the neurotoxic actions of estrogen in developing cerebellar neurons [J]. Toxicol Lett, 2008, 176(2): [11] Silva AS, Freire JMC, García RS, et al. Time temperature study of the kinetics of migration of DPBD from plastics into chocolate, chocolate spread and margarine [J]. Food Res Int, 2007, 40(6): [12] Silva AS, Freire JMC, Franz R, et al. Time-temperature study of the kinetics of migration of diphenylbutadiene from polyethylene films into aqueous foodstuffs [J]. Food Res Int, 2008, 41(2): 作者简介 ( 责任编辑 : 白洪健 ) 王颖, 主管技师, 主要研究方向为食品检验 [email protected] 孙兆鹏, 主管技师, 主要研究方向为食品检验 @qq.com

Microsoft Word - 20120928-275_editing.doc

Microsoft Word - 20120928-275_editing.doc GC-FID 法测定塑料包材中 16 种邻苯二甲酸酯类化合物杨瑛, 樊文娟 ( 廊坊梅花生物技术开发有限公司, 河北廊坊 065001) 摘要 : 采用气相色谱 - 氢火焰离子化检测法对四种塑料包材中 16 种邻苯二甲酸酯类化合物进行测定该方法线