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1 4 5 Vol. 4 No Journal of Food Safety and Quality Oct., 白 1, 爽 2, 李英 1*, 金文标 2, 廖文忠 1, 陈旭辉 1, 李泳涛 1, 梁烽 李成发 1, 陈麒宇 1, 孙小颖 1 1, (1., ; 2., ) 摘要 : 目的 方法, - (gas chromatography-mass spectrometry, GC-MS) 结果 ~10 μg/l, R μg/l 3, % 119.8%, 0.99% 15.93% 结论, 关键词 : ; - ; Determination of polycyclic aromatic hydrocarbons in alcohol food simulation by gas chromatography-mass spectrometry BAI Shuang 1, 2, LI Ying 1*, JIN Wen-Biao 2, LIAO Wen-Zhong 1, CHEN Xu-Hui 1, LI Yong-Tao 1, LIANG Feng 1, LI Cheng-Fa 1, CHEN Qi-Yu 1, SUN Xiao-Ying 1 (1. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen , China; 2. Shenzhen Graduation School, Harbin Institute of Technology, Shenzhen , China) ABSTRACT: Objective To develop a method for the determination of polycyclic aromatic hydrocarbons (PAHs) in alcohol food simulation by chromatography-mass spectrometry (GC-MS) using solid phase microextraction (SPME). Methods The experimental conditions of SPME, such as extraction mode, extraction temperature, extraction time, desorption time and agitation speed were optimized. Qualitative and quantitative analysis were carried out by total ion chromatogram and selected ion chromatogram with GC-MS. Results The method showed a good linearity in the range of 0.01~10.00 μg/l for PAHs with R 2 >0.99. Average recoveries of PAHs were 76.52%~119.8% with relative standard deviation of 0.99%~15.93% at three fortification levels of 0.1, 0.5, and 1.0 μg/l. Conclusion This method is simple, sensitive, and accurate, and it is suitable for the determination of PAHs in 10% alcohol food simulation. KEY WORDS: polycyclic aromatic hydrocarbons; gas chromatography-mass spectrometry; alcohol food simulation 基金项目 : (SZ ) Fund: Supported by Shenzhen Entry-Exit Inspection and Quarantine Bureau (SZ ) * 通讯作者 :,, ccibly@126.com *Corresponding author: LI Ying, Senior Engineer, Shenzhen Entry-Exit Inspection and Quarantine Bureau, No.289, Gongye 8th Rd. Nanshan District, Shenzhen , China. ccibly@126.com

2 5, : , [1-4], (polycyclic aromatic hydrocarbons, PAHs), [5], [6,7] [8-13], [14] [15-17] [18],, Pawliszyn [19],,, [20-25] GC-MS, 1 材料与方法 1.1 仪器与试剂 Agilent7890A-5975C / ( ) CTC Combi PAL ; DELTA320A ph ( ); 100 µm (PDMS) 16 PAHs (, 100 mg/l, Supelco ); ( ); ( ); ( Millipore, 18.2 MΩ cm) PAHs : PAHs, 20 mg/l 10%, 10%( ) : 100 ml 1 L, 1.2 分析条件 : HP-5MS : 30 m 0.25 mm i.d., 0.25 μm; : 60, 10 /min 260, 2 /min 280, 10 min; 280 ; He( %); 1.0 ml/min; : EI; 70 ev; 150 ; : 230 ; : 280 ;, ; min, ; min; m/z 128; min, m/z 152,153,165; min, m/z 178; min, m/z 202; min, m/z 228; min, m/z 252; min, m/z 276, 实验方法 10% GB/T [26], 4 10% 18 ml,, (solid phase microextraction, SPME), SPME, 45 ( 250 r/min) 30 min - (gas chromatography-mass spectrometry, GC-MS), min 2 结果与分析 2.1 定性 定量分析 (selected ion monitoring, SIM),,, 16,, 1.3, SIM 1 ( 1), 2.2 萃取方式的选择 (direct immersion-solid phase microextraction, DI-SPME) (headspace solid phase micro-extraction, HS-SPME),

3 Table 1 表 1 16 种多环芳烃的名称 CAS 号 分子式 分子量及特征离子 Names, CAS No., moleculer formula, molecular weight and characteristic ions of 16 PAHs CAS No. /amu /min 1 naphthalene C 10 H ,128, acenaphthylene C 12 H ,152, acenaphthene C 12 H ,153, fluorene C 13 H ,166, phenanthrene C 14 H ,178, anthracene C 14 H ,178, fluoranthene C 16 H ,202, pyrene C 16 H ,202, [a] benzo[a]anthracene C 18 H ,228, chrysene C 18 H ,228, [b] benzo[b]fluoranthene C 20 H ,252, [k] benzo[k]fluoranthene C 20 H ,252, [a] benzo[a]pyrene C 20 H ,252, [1,2,3-cd] indeno[1,2,3-cd]pyrene C 20 D ,276, [a,h] dibenzo[a,h]anthracene C 22 H ,278, [g,h,i] 苝 ( ) benzo[g,h,i]perylene C 22 H ,276, % 16 Fig. 1 Selected ion monitoring chromatogram of 16 PAHs in 10% ethanol simulation,, 10%,,, 2.3 解吸条件的选择, μg/l

4 5, : , min, 2, 4 min 2.4 萃取条件的优化 萃取时间,, 2 2,, 1# ; 2# 6#, 20 min ; 7# 16#, 50 min, 30 min 萃取温度, 16 ( 3),, 1# 6# ; 7# 8# ; 9# 11# ; 12# 16# 50, 16, 45 2 SPME 16 (10% ) Fig. 2 Effect of SPME time on the absorption of 16 PAHs (10% ethanol simulation) Fig. 3 3 SPME (10% ) Effect of extraction temperature on the absorption of PAHs(10% ethanol simulation)

5 振荡速度,, 250 r/min, ; 500 r/min,, 750 r/min,, 250 r/min 2.5 线性范围和检出限 ( )(20 mg/l), 10%( ), μg/l, Y X(μg/L),, 0.01 μg/l 10 μg/l, R μg/l(s/n=3) 2.6 精密度及回收率 µg/l (n=5), 10% % 15.93%,, - ( 60 ; 0.5 h) ( 60 ; 0.5 h) ( 95 ; 0.5 h) 3,,, , 10% %~119.8% 3 结论, GC/MS, - (SPME-GC/MS),, 参考文献 [1],. [J]., 1995, (9): Liu SQ, Wang P. Polycyclic aromatic hydrocarbons in the environment and carcinogenicity [J]. Environ Prot, 1995, (9): [2] ZEK (AtAV), 2011[Z]. ZEK The German federal work with technical equipment and consumer product commission, 2011 [Z]. [3]. [M]. :, 2001: Yang RM. Poisonous and harmful chemicals in the environment pollution and monitoring [M]. Beijing: Press of Minzu University of China, 2011: [4],,,. [J]. :, 2009, 45(2): Xiao HQ, Wang X, Wang C, et al. GC MS determination of polycyclic aromatic hydrocarbons in plastics [J]. PTCA (Part B: Chem Anal), 2009, 45(2): [5],. [M]. :, 2009, 22(6): Yang FX, Wu LQ. New practical material and new technology of Food packaging (The second edition) [M]. Beijing: Chemical Industry Press, 2009, 22(6): [6],,. [J]., 37(10): XI QH, ZHANG J, SHEN H. Migration rule of polycyclic aromatic hydrocarbons in food contact materials to food simulants [J]. Food Sci Technol, 37(10): [7],,,. (a) [J]., 2011, 31(3): Lin LR, Luo HD, Zhou N, et al. Determination of migration level of benzo(a) pyrene from paper cups into food simulants [J]. Spectrosc Spect Anal, 2011, 31(3): [8] Jonker T, Koelman SA. Extraction of polycyclic aromatic hydrocarbons from soot and sediment: solvent evaluation and implications for sorption mechanism [J]. Environ Sci Technol, 2002, 36(19): [9] Buco S, Moragues M, Doumenq P, et al. Analysis of polycyclic aromatic hydrocarbons in contaminated soil by curie point pyrolysis coupled to gas chromatography mass spectrometry, an alternative to conventional methods [J]. J Chromatogr A, 2004, 1026(1):

6 5, : [10],,,. 16 [J]., 2009, 27(3): Liu WZ, Gao YJ, Liu S, et al. Determination of 16 polycyclic aromatic hydrocarbons in food contact printing ink [J]. J Prev Med Chin PLA, 2009, 27(3): [11]. [D]., Li M. Solid phase extraction and HPLC for analysis of trace organic pollutants in environmental water samples [D]. Qingdao Technology University. [12],,,. / 16 [J]., 2012, 30(5): Tang ZW, Xie GX, He LF, et al. Determination of polycyclic aromatic hydrocarbons in water samples using solid phase extraction coupled with gas chromatography mass spectrometry [J]. J Longyan Univ, 2012, 30(5): [13],,. [J]., 2012, 28(6): Huang SJ, Wang YJ, Xu ZC. Determination of polycyclic aromatic hydrcarbons and phthalic acid esters in drinking water by solid phase extraction gc ms/ms [J]. J Anal Sci, 2012, 28(6): [14],,,. [J]., 2009, 30(1): 43 45, 64. Mao MY, Liu SQ, Song L, et al. Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Plastic Food Packaging [J]. Packaging Eng, 2009, 30(1): 43 45, 64. [15] SN/T [S]. SN/T Food contact materials Auxiliary materials Determination of polycyclic aromatic hydrocarbons (PAHs) in ink Gas chromatography/mass spectrometry [S]. [16] SN/T [S]. SN/T Food contact materials Wax Determination of polycyclic aromatic hydrocarbons in food simulants [S]. [17] SN/T [S]. SN/T Food contact materials Wood materials Determination of polycyclic aromatic hydrocarbons in food simulants [S]. [18] SN/T [S]. SN/T Food contact materials and articles Determination of PAHs in plastics and plastics items HPLC method [S] [19]. [M]. :, 2012: 2. Wu CY. Solid Phase Micro Extraction [M]. Beijing: Chemical Industry Press, 2012: 2. [20],,. SPME HPLC [J]., 2011, 27(7): Liu Y, Yang FW, Yang LJ. Determination of PAH by Solid phase Microextraction Coupled to HPLC Using Fibers with Mesoporous Coating [J]. Resour Dev Market, 2011, 27(7): [21],,. 16 [J]., 2008, 27(1): Luo SX, Zhu HW, Zhang XY. Solid phase Microextraction Coupled with Gas Chromatography for the Analysis of 16 Polycyclic Aromatic Hydrocarbons in Drinking Water Sources [J]. J Agr Environm Sci, 2008, 27(1): [22] Liu Y, Lee LM. Solid phase microextraction of PAH from aqueous samples using fibers Coated with HPLC chemically bonded silica stationary phases [J]. Anal Chem, 1997, 69(24): [23] Li QL, Xu XQ, Sen Chun LF, et al. Determination of trace PAHs in seawater and sediment pore water by solid phase microextraction (SPME)coupled with GC/MS [J]. Sci China Ser B: Chem, 2006, 49(6): [24] Guillén MD, Sopelana P. Headspace solid phase micro extraction as a tool to estimate the contamination of smoked cheeses by polycyclic aromatic hydrocarbons [J]. J Dairy Sci, 2005, 88(1): [25],,,. [J]., 2008, 29(6): Chen DW, Wang F, Meng SN, et al. Study on extraction of polycyciic aromatic hydrocarbons from smoked meat by MAE SPME [J]. Sci Technol Food Ind, 2008, 29(6): [26] GB/T [S]. GB/T Materials and articles in contact with foodstuffs Plastics substances subject to limitation Guide to test methods for the specific migration of substances from plastics to foods [S]. ( 责任编辑 : 赵静 )

7 作者简介 白爽, 大学, 工程师, 主要研究方向为材料检测技术 baishuang1981@126.com 李英, 硕士, 研究员, 主要研究方向为色谱检测技术 ccibly@126.com 食品中持久性有机污染物研究 专题征稿 投稿方式 : 食品安全质量检测学报 编辑部