Microsoft Word _二校出3711,3714,3715

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1 7 9 Vol. 7 No Journal of Food Safety and Quality Sep., * 田良良, 于慧娟, 孔聪, 韩峰, 黄冬梅, 王媛, 蔡友琼 (, ( ), ) 摘要 : 目的 - 7 方法, - (1:1, V:V), 120, 10 MPa, 8 min, 2, 结果 5~500 ng/ml, ~0.9999, 3.0~5.0 μg/kg, %~104%, 2.61%~8.26% 结论,,, 关键词 : ; ; ; Study on the method for detecting 7 kinds of indicative polychlorinated biphenyls in fish meal by accelerated solvent extraction-gas chromatography TIAN Liang-Liang, YU Hui-Juan, KONG Cong, HAN Feng, HUANG Dong-Mei, Wang Yuan, CAI You-Qiong * (Aquatic Product Quality Inspection and Test Center(Shanghai), Ministry of Agriculture of PR China, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai , China) ABSTRACT: Objective To establish a method for detecting 7 kinds of indicative polychlorinated biphenyls (PCBs) residues in fish meal by accelerated solvent extraction-gas chromatography (ASE-GC). Methods The PCBs were extracted with n-hexane-methylene chloride (1:1, V:V) by ASE with the extraction temperature at 120, pressure at 10 MPa, and the static extracting time at 8 min. The above operating steps were repeated twice. After being purified by concentrated sulfuric acid, the extract was analyzed by GC. Results The PCBs had good linearities at the range of 5~500 ng/ml, the correlation coefficients were ~0.9999, and the limit of quantification were 3.0~5.0 μg/kg. The average recovery rates of the PCBs in 3 spiked levels ranged from 85.5% to 104% with the relative standard deviations (RSDs) were 2.61%~8.26%. Conclusion The proposed method was precise, accurate, simple and rapid, which is suitable for the quantitative detection of PCBs in fish meal. KEY WORDS: fish meal; polychlorinated biphenyls; accelerated solvent extraction; gas chromatography 基金项目 : (2014T14) Fund: Supported by Special Research Fund for the National Non-Profit Institutes (2014T14) * 通讯作者 :,, caiyouqiong@163.com *Corresponding author: CAI You-Qiong, Professor, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai , China. caiyouqiong@163.com

2 9, : 引言 (polychlorinated biphenyls, PCBs), 12,, [1,2] PCBs, PCBs 90% [3],,,,,, [4],, PCBs (accelerated solvent extraction, ASE),,,, [5], [6] ASE [5], [7] [8] [9,10] [6,11], [6,12,13] [14,15] Pu Wang [5] ASE, ASE,, [16] (Soxhlet) [17],, 24 h,, PCBs, PCBs (gas chromatography, GC) -(gas chromatography-mass spectrography, GC/MS), GC,, GC 2 材料与方法 2.1 材料与试剂 PCB28 PCB52 PCB101 PCB118 PCB138 PCB153 PCB180 PCB198( 98%, Dr.Ehrenstorfer ); (, J.T.Baker ); (, J.T.Baker ); (, ) 2.2 仪器与设备 7890N ( 7683 ECD, Agilent ); APLE-3000 (); RE-52A ( ) 2.3 实验方法样品处理, 40, 3.00 g 1.6 g, 50 ng PCB198,, 11 ml, 30 min ASE : - (1:1, V/V), 30 s, 10 MPa, 120, 5 min 8 min, 60%, 90 s, 样品提取液的净化, 6 ml 2, 10 ml ; 2 ml, 2000 r/min 5 min;, 3 ml,, ; 1 ml,,,,, ;, 1 ml, GC 气相色谱分析 DB-17MS ((50%- )-, 30 m 0.32 mm, 0.25 μm); 280, 300 ;, 0.75 min, 1.2 ml/min, 1 μl : 150, 15 /min 200, 2 /min 270, 2 min; 10 /min 280, 1 min 标准曲线的绘制 : PCB28 PCB52 PCB101 PCB118 PCB138 PCB153 PCB mg, 100 ml, 100 μg/ml, ng/ml 7 (PCB ng/ml),,, ⑴ PCBs : X C V (1) m :

3 食品安全质量检测学报第7卷 X: 样品中相应的 PCB 的残留量, µg/kg; 速率加快[18], 但同时必须保证此温度下提取溶剂为液态才 V: 样品溶液总体积, ml; 可以使实验进行实验结果表明, 随着温度的升高, 多氯联 C : 样品溶液中相应的 PCB 的浓度, ng/ml; 苯的外标回收率相应升高(图 1), 当提取温度为 120 时, 7 m : 样品质量, g 种多氯联苯的外标回收率都大于 95%, 且在实验选取的几种温度条件下最高温度再升高至 140 时的回收率比结果与分析 120 时的回收率增加已不明显, 甚至在某些样品 (PCB118 PCB138 和 PCB180)中有所下降, 这可能是由于提取溶剂的选择提取溶剂的种类是根据目标物的性质来决定的本实验选用正己烷-丙酮(1:1, V/V)和正己烷-二氯甲烷(1:1, V/V) 作为提取溶剂分别进行实验, 发现二者对 7 种指示性多氯在一定的压力下, 温度过高时化合物容易挥发造成的 [19], 故本研究选用 120 作为提取温度 3.3 提取时间的选择联苯的回收率均大于 85%, 但当提取溶剂为正己烷-二氯提取时间对 ASE 提取效率的影响也比较明显延长甲烷(1:1, V/V)时, 样品图谱中的杂峰更少, 所以选择正己提取时间可以提高回收率, 但是会浪费溶剂和时间实验烷-二氯甲烷作为提取溶剂结果表明, 随着提取时间的增加, 多氯联苯的外标回收率提取温度的优化也相应增加(图 2), 当萃取时间为 8 min 时, 多氯联苯的回温度是影响 ASE 提取效率的关键因素, 在一定压力收率均大于 90%, 再增加萃取时间, 对回收率的增加无明 3.2 下, 提高温度可以使被提取物的溶解度增加, 溶质的扩散 Fig. 1 显影响, 所以将 8 min 作为提取时间图 1 提取温度对回收率的影响 Effect of extraction temperature on the recovery Fig. 2 图 2 提取时间对回收率的影响 Effect of extraction time on the recovery

4 9, : 加速溶剂萃取循环次数的确定,, 2 3 [20],,, 7 70%; 2, 90%; 3 2 5%, 净化方式的优化 ASE,,,, 3 ml 2 ( 3), 3.6 标准曲线的绘制 2.3.3,,,, S/N( ) 3, S/N 10, 回收率和精密度实验, μg/kg, 6,, 2 2, 3, 85.5%~104%, (relative standard deviation, RSD) 2.61%~8.26%,, 3 (A) (B) Fig.3 Chromatograms of PCBs standard(a) and a spiked fish meal sample(b) Table 1 表 1 多氯联苯的回归方程线性范围相关系数方法检出限和定量限 Linear equations, linear ranges, correlation coefficients(r), detection limits, and quantization limits of PCBs (ng/ml) (r) (μg/kg) (μg/kg) PCB28 Y=0.4581X ~ PCB52 Y=0.2604X ~ PCB101 Y=0.3809X ~ PCB118 Y=0.4533X ~ PCB153 Y=0.4201X ~ PCB138 Y=0.6398X ~ PCB180 Y=0.6790X ~

5 表 2 Table 2 多氯联苯的回收率 (n=6) The recoveries of PCBs (n=6) : 5 μg/kg : 20 μg/kg : 50 μg/kg (μg/kg) RSD (μg/kg) RSD (μg/kg) RSD PCB PCB PCB PCB PCB PCB PCB 样品测定 4,, 结论 ASE 7,, ASE,,, PCBs 参考文献 [1] Andersson PL, Berg AH, Bjerselius R, et al. Bioaccumulation of selected PCBs in zebrafish, three-spined stickleback, and arctic char after three different routes of exposure [J]. Arch Environ Con Tox, 2001, 40(4): [2] Smith AG, Gangolli SD. Organochlorine chemicals in seafood: occurrence and health concerns [J]. Food Chem Tox, 2002, 40(6): [3]. [M]. :, Wu YN. Modern Food Safety Science [M]. Beijing: Chemical Industry Publisher, [4]. [J]., 2010, (9): Chen HL. The research progress of toxic ingredients in fishmeal [J]. Hubei J Anim Vet Sci, 2010, (9): [5] Richter BE, Jones BA, Ezzell JL, et al. Accelerated solvent extraction: a technique for sample preparation [J]. Anal Chem, 1996, 68(6): [6] Wang P, Zhang QH, Wang YW, et al. Evaluation of Soxhlet extraction, accelerated solvent extraction and microwave-assisted extraction for the determination of polychlorinated biphenyls and polybrominated diphenyl ethers in soil and fish samples [J]. Anal Chim Acta, 2010, 663(1): [7] Aroclor [J]., 2014, 30(2): Pan Y. Simultaneously determination of seven kinds of aroclor in soil by accelerated solvent extraction and gas chromatography mass spectrometry [J], Environ Monit China, 2014, 30(2): [8],. -[J]., 2015, 32(1): Zhang Y, Chen YM. Determination of polychlorinated biphenyls in sediment by gas chromatography [J]. Stud Trace Elements Health, 2015, 32(1): [9],,, [J]., 2014, (1): Wang ZZ, Xu HY, Wang W, et al. Determination of 15 polychlorinated biphenyls in sediment by accelerated solvent extraction-gas chromatography [J]. J Anal Sci, 2014, (1): [10] Zhang P, Ge LK, Zhou CG, et al. Evaluating the performances of accelerated-solvent extraction, microwave-assisted extraction, and ultrasonic-assisted extraction for determining PCBs, HCHs and DDTs in sediments [J]. Chin J Oceanol Limn, 2011, 29(5): [11] Sporring S, Bøwadt S, Svensmark B, et al. Comprehensive comparison of classic Soxhlet extraction with Soxtec extraction, ultrasonication extraction, supercritical fluid extraction, microwave assisted extraction and accelerated solvent extraction for the determination of polychlorinated biphenyls in soil [J]. J Chromatogr A, 2005, 1090(1 2): 1 9. [12],,,. [J]., 2005, 15(10): Tie XW, Shen HT, Han JL, et al. Research of the PCBs pollution in freshwater fish in parts of Zhejiang province [J]. Chin J Health Lab Technol, 2005, 15(10): [13] 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, 142(1): [14],,,. [J]., 2005, 24(5):

9, : - 7 3715 Zhou L, Shen YH, Chen DZ, et al. Comparison of two pretreatment techniques for extraction of PCBs from mussels [J]. J Instrum Anal, 2005, 24(5): 43 46. [15],,,. - [J].

6 9, : Zhou L, Shen YH, Chen DZ, et al. Comparison of two pretreatment techniques for extraction of PCBs from mussels [J]. J Instrum Anal, 2005, 24(5): [15],,,. - [J]., 2006, 16(9): Fu WS, Lin Q, Lv HD, et al. Determination of polychlorinated biphenyls (PCBs) in foodstuffs by the isotope dilution GC -LRMS coupled with accelerated solvent extraction(ase) [J]. Chin J Health Lab Technol, 2006, 16(9): [16]. (PCBs) [J]., 2008, (18): Lan MZ. Determination of polychlorinated biphenyls (PCBs) residues in fish feed by gas chromatography [J]. Feed China. 2008, (18): [17] GB/T [S]. GB/T The national standard of the People's Republic of China [S]. [18],,,. [J]., 2014, 35(1): Niu GG, Deng JC, Li LH, et al. Accelerated solvent extraction and its applications in food analysis [J]. Sci Technol Food Ind, 2014, 35(1): [19] Wu G, Bao XX, Zhao SH, et al. Analysis of multi-pesticide residues in the foods of animal origin by GC-MS coupled with accelerated solvent extraction and gel permeation chromatography cleanup [J]. Food Chem, 2011, 126(2): [20] Bjo rklund E, Bøwadt S, Nilsson T, et al. Pressurized fluid extraction of polychlorinated biphenyls in solid environmental samples [J]. J Chromatogr A, 1999, 836(2): 作者简介 ( 责任编辑 : 刘丹 ) 田良良, 助理研究员, 主要研究方向为水产品质量安全 liangliangjia@126.com 蔡友琼, 研究员, 主要研究方向为水产品质量安全与控制 caiyouqiong@163.com

Microsoft Word 吴益春

Microsoft Word 吴益春 6 3 Vol. 6 No. 3 2015 3 Journal of Food Safety and Quality Mar., 2015 - 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., 316000; 2., 316000; 3., 3160) 1,2, 摘要 : 目的 - 方法, + (:, v:v) 结果 GBW(E)0131,,

Microsoft Word _二校 出3711,3714,3715

Microsoft Word _二校出3711,3714,3715