Microsoft Word 吴益春

Transcription

1 6 3 Vol. 6 No Journal of Food Safety and Quality Mar., 吴益春 1,2, 祝世军 1,2, 罗海军 1,2, 陈璐 1,2, 鲁华郭海波 1,2, 杨会成 3 1*, 郝云彬 (1., ; 2., ; 3., 3160) 1,2, 摘要 : 目的 - 方法, + (:, v:v) 结果 GBW(E)0131,, 93.7%~4.4%, 2.75%~4.65%, 0.22~0.44 µg/kg 结论,, 关键词 : ; ; ; Determination of indicator polychlorinated biphenyls residues in the flesh of fish by gas chromatography using acid digestion WU Yi-Chun 1,2, ZHU Shi-Jun 1,2, LUO Hai-Jun 1,2, CHEN Lu 1,2, LU Hua 1,2, GUO Hai-Bo 1,2, YANG Hui-Cheng 3, HAO Yun-Bin 1* (1. Zhoushan Fisheries Test Center, Zhoushan , China; 2. Zhoushan Institute for Food and Drug Control, Zhoushan , China; 3. Zhejiang Marine Development Research Institute, Zhoushan 3160, China) ABSTRACT: Objective To establish a method to detect the residual indicator polychlorinated biphenyls (PCBs) in the flesh of fish by gas chromatography using acid digestion. Methods The sample was digested by H 2 SO 4, then extracted by N-hexane and methylene chloride (:, v:v) and cleaned up by H 2 SO 4, after that determined by capillary gas chromatography. Results PCBs reference material GBW(E)0131 in Cod was detected by this method and the result was in accordance with the assigned value. The recovery was 93.7%~4.4%, RSD was 2.75%~4.65% (n=6), and the detection limit was 0.22~0.44 µg/kg. Conclusion The method is simple, rapid, sensitive, accurate and precise, and it can be used for the determination of indicator polychlorinated biphenyls in the flesh of fish. KEY WORDS: flesh of fish; polychlorinated biphenyls; acid digestion; gas chromatography 基金项目 : (2012BAD29B06) Fund: Supported by National Support Program for Science and Technology (2012BAD29B06) * 通讯作者 :,, yunbinhao@163.com *Corresponding author: HAO Yun-Bin, Senior Engineer, Zhoushan Fisheries Test Center, Zhoushan, No.55, Jinsha Road, Putuo District, Zhoushan , China. yunbinhao@163.com

2 引言 (polychlorinated biphenyls, PCBs),, PCBs,,,,, [1-5], PCBs [6-13] PCBs,, PCBs, [6] [6] [7] [8] [9,] [11,12] R134a [13] GB [6], ( 18~24 h),,, ; R134a,, R134a,,,,,, PCBs [14],,, ( PCB28 PCB52 PCB1 PCB118 PCB153 PCB138 PCB180) 2 材料与方法 2.1 试剂与仪器 (, Fisher Scientific ); (, ); (, ); (, Fisher Scientific ); (, ):,, 225 ; (, ): h PCBs (7, 28, 52, 1, 118, 138, 153, 180), o2si ; (GBW(E)0131, ) Agilent 7890A, ( ); (RV, IKA ); (CT14D, ); (IP40, IKA ) 2.2 样品前处理 5 g ( 0.01 g) ml, 12 ml %, 80 1 h, ml + (:, v:v), 2 min, 5 min,, ml, ml, ml, ml, 1 min, 7000 r/min 1 min,,, ( 2.5 g 2 g, 15 ml ), 0 ml, 30 ml, 25 ml + (5:95, v:v), 40 1 ml, 2.3 色谱条件 : HP-5MS(Crolinked 5% Pheny1 Methy1 Siloxane, 30 m 0.32 mm, 0.25 µm) : 290 ;, : 300 ; : min, 15 /min 200, 5 min; 3 /min 2, 2 min; : 60 ml/min 2.4 计算公式与数据处理, :

3 3, : = PCBs / PCBs 0% SPSS 13.0,, P< 结果与分析 3.1 酸消化时间的选择 %, 5, 1 %, 0.5 h, 42.4%~65.0%, 1.0 h, 93.7%~4.4%,,, % 1.0 h,,,, 表 1 不同消化时间对提取率的影响 (n=5) Table 1 Effect of different incubation time on extraction efficiency(n=5) (%) 0.5 h 1 h 2 h 3 h PCB ± ± ± ±4.05 PCB ± ± ± ±5.75 PCB1 65.0± ± ± ±3.82 PCB ± ± ± ±2.16 PCB ± ± ± ±3.78 PCB ± ± ± ±3.52 PCB ± ± ± ± 萃取用试剂的选择, [2], 2, + (:, v:v), (P<0.05), + (:, v:v) Table 2 表 2 不同萃取试剂对提取率的影响 Effect of different incubation time on extraction efficiency (%) + (:, v:v) + (:, v:v) PCB ± ± ± ±4.19 PCB ± ± ± ±2.98 PCB1 62.0± ± ± ±3.98 PCB ± ± ± ±3.74 PCB ± ± ± ±4.82 PCB ± ± ± ±2.92 PCB ± ± ± ± 色谱柱的选择, : HP-35 PCB123 PCB118,, HP-5MS, [15] 7 1 Fig (80 ng/ml) Chromatogram of 7 kinds of PCBs in samples (80 ng/ml)

4 线性回归方程 检出限与定量限 ng/ml,,, 3, , 0.22~0.44 µg/kg, 0.5 µg/kg 3.5 回收率和精密度试验 0 µg/kg 7,,, 93.7%~4.4%, (RSD, n=6) 2.75%~4.65%, 4 表 3 7 种 PCBs 的线性关系及其检出限 Table 3 Regression equations and detecting limits of 7 kinds of PCBs PCB (min) R (µg/kg) PCB Y= X PCB52.9 Y= X PCB Y= X PCB Y= X PCB Y= X PCB Y= X PCB Y= X 表 4 鲳鱼样品中添加多氯联苯回收率和精密度 (n=6) Table 4 Recoveries and relative standard deviations (RSDs) of PCBs adding in Pomfret (n=6) /(µg/kg) /% RSD/% PCB28 PCB52 PCB1 PCB118 PCB153 PCB138 PCB

5 3, : - 927, 样品检测结果 ( ) ( : GBW(E)0131), 3,, 5 5,, RSD 5% 表 5 标准物质中多氯联苯检测结果 (n=3) Table 5 The PCBs content in sample(n=3) (ng/g) (ng/g) (%) ( ) (ng/g) (%) PCB ± % PCB ± % PCB1 40.5± % PCB ± % PCB ± % PCB ± % PCB ± % 结论, ( ), [3] 18~24 h, 3~4 h,, 0~200 µg/l,, , 93.7%~4.4%, RSD 5%,, 参考文献 [1] Maria Maddalena Storelli, Grazia Barone, Veronica Giuliana Perrone, et al. Polychlorinated biphenyls(pcbs), dioxins and furans(pcdd/fs): Occurrence in fishery products and dietary intake [J]. Food Chem, 2011, 127(4): [2] Gemma Perelló, Roser Martí-Cid, Victoria Castell, et al. Influence of various cooking processes on the concentrations of PCDD/PCDFs, PCBs and PCDEs in foods [J]. Food Control, 20, 21(2): [3] Ottonello G, Ferrari A, Magi E. Determination of polychlorinated biphenyls in fish: optimisation and validation of a method based on accelerated solvent extraction and gas chromatography-mass spectrometry [J]. Food Chem, 2014, 1(142): [4] Bocio A, Domingo JL, Falcó G, et al. Concentrations of PCDD/PCDFs and PCBs in fish and seafood from the Catalan (Spain) market: estimated human intake [J]. Environ Inter, 2007, 33(2): [5],. [J]., 2004, 16(6): Li JG, Wu YN. Progress in press in pretreatment for determination of polychlorinated biphenyls from food matrices [J]. Chin J Food Hyg, 2004, 16(6): [6] GB [S]. GB National food safety standards determination of indicator polychlorinated biphenyls in foods [S]. [7],,,. - 7 [J]., 2011, 45(6): Ma LS, ZHU XP, Zheng GM, et al. Determination of seven kinds of polychlorinated biphenyls in aquatic products by matrix solid-phase dispersion and gas chromatography [J]. Chin J Vet Drug, 2011, 45(6): [8],,,. [J]., 2014, 42(14): Sun XM, Hu HM, Zhong Z, et al. Determination of polychlorinated biphenyls and organochlorinated pesticides in mussel by gas chromatography [J]. Guangzhou Chem Ind, 2014, 42(14): [9],,,. - [J]., 2013, 32(1): Wu JH, Li A, Liu GY, et al. Determinaiton of polychlorinated biphenyls and organochlorine pesticide residues in wakame by gas chromatography with electron capture detection using microwave-assisted extraction [J]. Environ Chem, 2013, 32(1): [] Xiong GH, He XQ, Zhang ZX. Microwave-assisted extraction or saponification combined with microwave-assisted decomposition applied in pretreatment of soil or mussel sample for the

6 928 6 determination of polychlorinated b-iphenyls [J]. Anal Chim Acta, 2000, 413: [11],,,. - [J]., 2006, 16(9): Fu WS, Lin Q, Lu HD, et al. Determination of polychlorinated biphenyls ( PCB s) in foodstuffs by the isotope dilution GC- LRMS coupled with accelerated solvent extraction (ASE) [J]. Chin J Health Lab Technol, 2006, 16(9): [12] Mark M, Mary S, Karen T, et al. Simultaneous extraction of PCDD/PCDF and PCBs using accelerated solvent extraction for sediment, tissue and sludge matrices [J]. Organ Comp, 2003, 60: [13],,,. 7 - [J]., 2014, 26(2): 1 6. Wang TT, Li L, Chen YH, et al. Determination of 7 polychlorinated biophenyls in canned mackerel sub-critical water extraction-gas chromatography method [J]. J Ningbo Univ Technol, 2014, 26(2): 1 6. [14],,,. [J]., 2003, 12(2): Wang JH, Zhang YB, Lin LM, et al. Determination of the residual Polychlorinated biphenyls and organaochlorine pesticides in aquatic products [J]. Chem Anal Meterag, 2003, 12(2): [15],,. [J]., 2008, 29(7): Huang DM, Yu HJ, Sheng XS. Study on analytical method for trace polychlorobiphenyls in aquatic products [J]. Food Sci, 2008, 29(7): 作者简介 ( 责任编辑 : 杨翠娜 ) 吴益春, 硕士, 工程师, 主要研究方向为水产品质量安全 wmq728@126.com 郝云彬, 博士, 高级工程师, 主要研究方向为水产品质量安全 yunbinhao@163.com