Microsoft Word 陈志民-二校

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1 8 6 Vol. 8 No Journal of Food Safety and Quality Jun., 陈志民, 徐晓枫, 蒲云霞 *, 李伟, 单美娜, 刘宇 (, ) 摘要 : 目的 2013, 方法 ( (2- ) ) 结果 150, 46 (2- ), 30.67%; 18.67% 20.00%, mg/kg 0.85 mg/kg; 15, 10.00%,, 38.89%, 19.44% 结论,, 关键词 : ; ; ; Investigation and analysis of 3 kinds of phthalates esters in commercially available vegetable oils in Inner Mongolia area in 2013 CHEN Zhi-Min, XU Xiao-Feng, PU Yun-Xia *, LI Wei, SHAN Mei-Na, LIU Yu (Inner Mongolia Comprehensive Center for Disease Control and Prevention, Hohhot , China) ABSTRACT: Objective To understand the pollution situation of phthalates esters (PAEs) in commercially available vegetable oils in Inner Mongolia area in 2013, so as to provide basis for strengthening food safety supervision and management. Methods A total of 150 samples of vegetable oils with different brands were collected from several commodity circulation areas. The concentrations of 3 kinds of PAEs were determined by solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS). Results Totally 46 positive samples of vegetable oils were detected with the detection rate of 30.67%. The detection rates of dibutyl phthalate (DBP) and bis(2- ethylhexyl) phthalate (DEHP) were 18.67% and 20.00%, respectively. The maximum concentrations of DBP and DEHP were and 0.85 mg/kg, respectively. Besides, 15 excess samples of vegetable oils were detected, with the exceeding rate of DBP was 10.00%, and the maximum detection rate and exceeding rate of DBP in flaxseed oil were 38.89% and 19.44%, respectively. Conclusion There are high detection rates of DBP and DEHP in commercially available vegetable oils in Inner Mongolia area, and the exceeding rate of DBP are detected. Therefore, more attentions should be paid to strengthen the supervision of the production process of vegetable oils and the * 通讯作者 :,,, btlisa2008@163.com *Corresponding author: PU Yun-Xia, Master, Senior Technical Personnel, Inner Mongolia Comprehensive Center for Disease Control and Prevention, No.50, Erdos Sreet, Yuquan District, Hohhot , China. btlisa2008@163.com

2 6, : potential pollution in vegetable oils from packaging materials, and regular monitoring work should be carried. KEY WORDS: phthalates esters; vegetable oils; Inner Mongolia area; investigation and analysis 1 引言, (phthalates, PAEs),,, (2- ) (bis(2-ethylexyl)phthalate, DEHP),, PAEs,,,, [1-5] 2004 DEHP [6], (Scientific Committee on Food, SCF), DEHP (allowable daily intake, ADI) 50 μg/(kg d) [7],,, PAEs, DEHP (diisononyl phthalate, DINP) (dioctyl phthalate, DNOP) (dibutyl phthalate, DBP) (dimethyl phthalate, DMP) (diethyl phthalate, DEP) 6, (di-iso-decyl phthalate, DIDP) 6 1,, ( ), [8,9], PAEs (gas chromatography, GC) (high performance liquid chromatography, HPLC)- (gas chromatography- mass spectrometry, GC-MS) - (high performance liquid chromatography-mass spectrometry, HPLC-MS) [10-13] GC-MS HPLC-MS GC-MS 3 (DBP DEHP DINP),, 2 材料与方法 2.1 仪器与试剂 Agilent 7890A-5795C ( Agilent ) MS 3 basic ( IKA ) N-EVAP ( Organomation )(10 ml, ) HP-6019 ()( Thermo Scientific) SILICA/PSA (1.0 g/6 ml, Dikma ) : DINP D 4 -DBP D 4 -DEHP(>98.0%, Accustandard ); 16 PAEs (1000 μg/ml, Accustandard ); (, Merk ) 2.2 试验样品, , 2.3 试验方法样品前处理 0.5 g( g) 10 ml, 0.1 ml D 4 -DBP D 4 -DEHP, 6 ml, 1 min, 3000 r/min 5 min, SILICA/PSA, 5 ml 5 ml, 1~2 ml, 5 ml, 45,, 1.0 ml, GC-MS :, 色谱条件 : Hp-5MS (30 m 0.25 mm, 0.25 μm); : 60 1 min, 20 /min 220, 5 /min 290, 2 min, min; 260 ; (, ); 1 ml/min; : ; : 1 μl : (electron impact ion source, EI): 70 ev; : 230 ; : 300 ; : 5.0 min; : (selected ion monitoring, SIM) 标准溶液配制 : D 4 - D 4 - (2-),, 5.0 μg/ml

3 : DINP g,, mg/ml 1 ml DINP 10 ml,,, PAEs 100 μg/ml(dinp 1094 μg/ml); 1 ml 10 ml,, PAEs 10 μg/ml(dinp μg/ml) -18, DINP μg/ml, DBP DEHP : μg/ml 3 结果与分析 3.1 方法的线性范围和检出限 2.3.2,, 1, 3,, r 0.999, (limits of determination, LODs) 0.02~0.05 mg/kg (2.0 μg/ml) Fig. 1 The chromatogram of three kinds of phthalates esters (2.0 μg/ml) 3.2 回收率和精密度, mg/kg 3, 3, %~115% 88.2%~103.1% 93.4%~98.5%, (relative standard deviation, RSD) <10%,, 3.3 植物油中 PAEs 的总体检出情况 150, 46, 30.67%, 0.32 mg/kg, P DINP DBP DEHP 18.67% 20.0%, 46.5 mg/kg 0.85 mg/kg [8] : (2-)(DEHP) (DINP) (DBP) mg/kg, DBP 15, DEHP, 10.0%, [14-16] 2 (DBP DEHP), DBP DEHP, 8 150, DBP, 38.89%,, 17.65% 13.33% 11.11%, 4, 19.44% 14.71% 6.67% 11.11% DEHP, 44.44%,, 35.29% 27.78% 10.0%, DBP,,, mg/kg; P mg/kg mg/kg; DEHP 3 4 Table 1 表 1 质谱基本参数和方法检出限线性方程 Parameters for the mass spectrometric detection and method detection limits and linear equations (min) (m/z) (m/z) r LODs(mg/kg) DBP ,205 Y=1.36X DEHP ,279 Y=1.005X DINP ,167 Y= X

4 6, : Table 2 表 2 植物油中 3 种邻苯二甲酸酯加标回收率结果 (n=3) Recoveries of three kinds of phthalates esters in vegetable oils (n=3) 0.5 mg/kg 1.0 mg/kg 2.0 mg/kg (%) RSD (%) (%) RSD (%) (%) RSD (%) DBP DEHP DINP Table 3 表 3 DBP 在不同植物油中的检出率及检出浓度 Detection rates and concentrations of DBP in different types of vegetable oils ( ) (%) (%) (mg/kg) (mg/kg) P ~ ~ ~ ND ND 0.14~ ND ND ND ND ND ND ND 0.00 ND 2 ND ND ND ND ND 0.00 ND ~ : ND Table 4 表 4 DEHP 在不同植物油中的检出率及检出浓度 Detection rates and concentrations of DEHP in different types of vegetable oils (%) (%) (mg/kg) (mg/kg) P ND ND 0.21~ ND ND 0.12~ ND ND 0.15~ ND ND 0.17~ ND ND ND ND ND ND ND ND ND 3 ND ND ND ND ND ND ND 2 ND ND ND ND ND ND ND ~ : ND 4 结论与讨论, , 46 DBP DEHP, 30.67% DBP DEHP 18.67% 20.00%, mg/kg 0.85 mg/kg DBP 15, 10.00%,

5 2344 8, 38.89%, 19.44%, [5,17], DBP DEHP,,, [5,18-20],,,,,,, PAEs 参考文献 [1],,,. [J]., 2011, 21(3): Wang YY, Guo CQ, Zhou HP, et al. Recent progress for application of phalate esters [J]. Plast Packag, 2011, 21(3): [2],,. [J]., 2005, 26(12): Cai J, Chai LY, Hu QH. Detection and safety evaluation of phthalic acid esters in food [J]. Food Sci 2005, 26(12): [3]. [J]., 2004, 26(19): Liu HJ. Toxicological effect and risks of phthalate acid esters on the health of population [J]. Acta Acad Med Mil Tert, 2004, 26(19): [4],,,. [J]. -, 2011, 47(2): Zhang LL, Chen HW, Li JQ, et al. Recent progress of methods for detection of phalate esters [J]. Phys Test Chem Anal Part B: Chem Anal, 2011, 47(2): [5],. [J], 2013, 38(5): 1 4. Cao JY, Jin QZ. Progress in contamination pathways and analysis methods of plasticizers in edible oil [J], China Oils Fats, 2013, 38(5): 1 4. [6]. [J]., 2012, 37(2): Guo YM. Toxicity and related restricted laws and regulations of phthalate esters [J]. Guangzhou Chem, 2012, 37(2): [7]. [M]. :, EU Regulations and Guidances on Food Contact Materials Editorial Board. EU regulations and guidances on food contact materials [M]. Beijing: Standards Press of China, [8]. ()[EB/OL]. [ ]. dcea6e. shtml. The Minister of Health of the People's Republic of China. Announcement of the list of potential illegal added nonfood substances and food additives abuse in food (part 6) [EB/OL]. [ ]. s7891/201106/39bee4fe171b4ec4b82df40b61dcea6e. shtml. [9],,, [J]. -, 2015, 51(6): LI N, Wang XN, Liu KS, et al. Determination of 7 phalate esteers in vegetable oil by GC-MS [J]. Phys Test Chem Anal Part B: Chem Anal, 2015, 51(6): [10],,,. 16 [J]., 2013, 23(2): Chen ZM, Xu XF, Ding YP, et al. Determination of 16 phthalate acid esters in edible oils [J]. Chin J Health Lab Technol, 2013, 23(2): [11]. 16 [J]., 2013, 35(6): Chen JH. Determination of 16 kinds of phthalate plasticizers in leather [J]. West Leather, 2013, 35(6): [12],,, [J]., 2015, 40(2): Zhang MM, Liu YL, Ma YX, et al. Determination of 7 kinds of phthalate acid esters in edible oil by solid-phase extraction-gas chromatography-mass spectrometry [J]. China Oils Fats, 2015, 40(2): [13],,. 17 [J]., 2016, 45(3): Du ZN, Miao HJ, Wu YN. Determination of 17 plasticizers in dairy food [J]. J Hyg Res, 2016, 45(3): [14] Fierens T, Servaes K, Van holderbeke M, et al. Analysis of phthalates in food products and packaging materials sold on the Belgian market [J]. Food Chem Toxicol, 2012, 50(7): [15],,, [J]., 2016, 43(14): Qin FG, Zou KT, Li YB, et al. Investigation and evaluation of phthalate esters in edible vegetable oils in Xi an in 2015 [J]. Mod Prev Med, 2016, 43(14): [16],,,. [J]., 2016, 7(10): Wang Y, Liu HY, Zhang GF, et al. Determination of plasticizers in finished and bulk oil in Yantai [J]. J Food Saf Qual, 2016, 7(10): [17],, [J], 2011, 32(10): , 446 Liu XY, Jiang KX, Shi WN. Evaluation Migratin of phthalates from food packing materials in and abroad. [J]. J Sci Technol Food ind, 2011, 32(10): , 446. [18],,,. [J]., 2016, 35(1): Zeng YX, Liang TT, Tang MH, et al. Migrating behaviors of phthalates

6, : 2013 3 2345 from food packing materials to simulant food [J]. J Mt Agric Biol, 2016, 35(1): 34 39. [19],,,. - [J]., 2016, 37(18): 146 151.

Food Sci, 2016, 37(18): 146 151. [20]. [J]., 2016, 16(36): 87 90. Liu XQ.

6 6, : from food packing materials to simulant food [J]. J Mt Agric Biol, 2016, 35(1): [19],,,. - [J]., 2016, 37(18): Hu AP, Liu YL, Zhang MM, et al. Direct determination of phthalate acid esters in oil feedstock by gas chromatography-mass spectrometry [J]. Food Sci, 2016, 37(18): [20]. [J]., 2016, 16(36): Liu XQ. Risk analysis and pollution control of phthalate esters in edible vegetable oil [J]. Mod Food, 2016, 16(36): ( 责任编辑 : 姜姗 ) 作者简介陈志民, 硕士, 主管检验师, 主要研究方向为食品安全风险检测 haiiang1218@163.com 蒲云霞, 硕士, 副主任检验师, 主要研究方向为食品安全风险检测与评估 btlisa2008@163.com

Microsoft Word 王颖-二校

Microsoft Word 王颖-二校 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%,