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1 5 4 Vol. 5 No Journal of Food Safety and Quality Apr., , 白艳艳 2, 谷伟丽 3 1,, 马元庆 2 1,, 孙珊 2, 魏潇 1, 张秀珍 (1., ; 2., ; 3., ) 1, 2* 摘要 : 目的 4 2, 方法, 4 ICP-MS2, 结果 3 (P>0.01), RSD%<2%, 101.2%~105.4%;, (P<0.01); -ICP-MS, 78.7% 结论, ;, ; -, ; -ICP-MS, 关键词 : ; ; ; Comparison of different preparation and determination methods of aluminum in jellyfish products BAI Yan-Yan 1, 2, GU Wei-Li 3, MA Yuan-Qing 1, 2, SUN Shan 1, 2, WEI Xiao 1 1, 2*, ZHANG Xiu-Zhen (1. Marine Resources and Environment Research Institute of Shandong Province, Yantai , China; 2. Shandong Provincial Key Laboratory of Restoration for Marine Ecology, Yantai , China; 3. Yantai Shanshui Seafood Co. Ltd, Yantai , China) ABSTRACT: Objective Four different pre-treatment methods combined with two different detection methods was established to determinate the aluminum content in jellyfish products to explore simple, precise, accuracy, strongly applicable detection method. Methods Fresh jellyfish, salted jellyfish and instant jellyfish samples were prepared by boiled digestion, acid digestion, microwave digestion and electric-heating-plate digestion respectively, and then aluminum content of each sample was determined using titration and ICP-MS methods, respectively. The precision and recoveries were measured simultaneously. Results There were no significant difference among 3 preparation approaches including acid digestion, microwave digestion and electric-heating-plate digestion with paired t-test (P>0.01). The recoveries were in the range of 101.2% 105.4% with RSD<2%. Significant difference was found between boiled digestion and the other 基金项目 : Fund: Supported by Ministry of Agriculture about Jellyfish Aluminum Safety Emergency Investigation * 通讯作者 :,, zxz @126.com *Corresponding author: ZHANG Xiu-Zhen, Professor, Marine Resources and Environment Research Institute of Shandong Province, No.216, Changjiang Road, Yantai , China. zxz @126.com

2 methods (P<0.01), and the recovery ratio was only 78.7% for acid digestion-icp-ms method. Conclusion Boiled digestion was not suitable for pretreatment of aluminum in jellyfish products with low extraction rate. Acid titration method could be used for the determination of jellyfish aluminum by enterprises and inspection agencies, with low costs, high precision and accuracy. Electric-heating-plate digestion plus titration method could be applied with satisfactory precision and accuracy to replace acid titration detection by the enterprises in case of a large quantity of samples. Microwave digestion plus ICP-MS method was suitable for research institutes of high standard facilities, because of its convenient operation, high sensitivity, and high recovery ratio. KEY WORDS: jellyfish products; aluminum; preparation; determination method 1 引言,, [1-7], [4] [5-7],, [2] WHO 1989 [8],, ( ) [7],,,,, [8-20], GB/T [10] S [12] [13], SC/T [9] [11] [14], [11] ICP-MS,, 2 材料与方法 2.1 仪器与试剂 DL-1 ( ); ( 0.01 ml, ); MARS ( CEM ); EH35B (LabTech ); ICP-MS 7500ce ( ) (); 0.6 mol/l ( ); 0.03 mol/l EDTA ( ); 1:1 ( ); 1:1 (); ( ); ( ); ); 0.5% ( ); (GBW(E)080219, 100 μg/ml); (GBW08620, 1000±1 μg/ml) milli-q 2.2 方法样品前处理方法, SC/T [9] 20 g,, 500 ml,,, [11] 0.6 mol/l 6 min, CEM MARS : ~120, 5 min, 120, 5 min; 120~160, 5 min,

3 4, : , 5 min; 160~180, 10 min, 180, 5 min 2~5 g( g), 10 ml,, 140~160, 50 ml, 3,, ;, LabTech EH35B : ~120, 120, 5 min; 180, 180, 2 h, 220 2~5 g( g), 10 ml,,,,,, 10 ml,, 50 ml, 3,, ; 样品检测方法,, SC/T [9] EDTA ICP-MS,, ICP-MS 7500ce 1, 2% µg/l 2.3 评价方法精密度计算, 回收率试验 mg/kg,, 数据统计方法 ANOVA Duncan, P< 结果与分析 3.1 不同前处理方法处理的样品状态 2 2,,, ;,,,, 表 1 ICP-MS 仪器工作条件 Table 1 Instrument parameters for ICP-MS 15.0 L/min 8.0 min 1.17 L/min W 0.1 s 2 3 Table 2 表 2 四种不同前处理方法的现象差异 Different pretreatment phenomena of 4 methods (g) 20 6 min,,,, 20 6 min,,, 2~5 1~2 h, 2~5 4~5 h,

4 不同检测方法测定结果的比较 ICP-MS, 3 3,, ICP-MS (P<0.01),,, ICP-MS ; ICP-MS (P<0.01), CI - H O Ar, Al,,,,, 8.17~8.82 mg/kg; 555~586 mg/kg; 377~415 mg/kg 3.3 方法精密度的比较, 4 4,, -ICP-MS RSD%, 6.59% 3.44%; ICP-MS RSD% 2%, 3.4 方法回收率的比较 8 5, -ICP-MS 78.7%, ICP-MS ;, 101.2%~105.4%, Table 3 表 3 不同检测方法铝的测定结果 Monitoring results of content of aluminum using different methods mg/kg mg/kg ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS 586

5 4, : 1201 Table 4 表 4 方法精密度比较 Comparison of precision of different determination methods n (mg/kg) RSD% ± ICP-MS ± ± ICP-MS ± ± ICP-MS ± ± ICP-MS ± Table 5 表 5 方法的加标回收率比较 Comparison of recoveries of determination methods mg/kg ICP-MS -ICP-MS -ICP-MS -ICP-MS 99.2~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 讨论 4.1 海蜇产品中铝的来源,, 2010 Al [14], 4.2 各种方法的特点,,,, Al, Al

6 1202 5,,,,,, ICP-MS,, ICP-MS,, ICP-MS,, 4.3 检测方法的适用性,, ; - -ICP-MS, 5 展望, GB ( 100 mg/kg(, Al )), SC/T [9], ;,, 参考文献 [1],,. 2011~2012 [J]., 2013, 4(2): Chen JW, Li H, Wang HL. Investigation and analysis of aluminum content in commercial foods in Rizhao city during 2011~2012[J]. J Food Safe Qual, 2013, 4(2): [2],. [J]., 2010, 24(21): Li QH, Li QF. Food contaminant survey of aluminum in Cangzhou [J]. Med Anim Contr, 2010, 26(11): [3],,,. [J]., 2012, (2): Tao RX, Zhang HJ, Jia DY, et al. The Progress of alum substitutes in processing of Sweet potato vermicelli[j].grain Feed Ind, 2012, (2): [4]. [A]// [C]. :, Niu Q. Neurotoxicity of aluminum [A]// The tenth national labor hygiene and occupation disease symposium [C]. Hangzhou: Chinese preventive medicine association, [5]. [J]. :, 2007, 9(1): Zheng X. Influence of aluminum to people s health and testing the content of aluminum food [J]. J Chongqing univ Sci Technol(Natural Sci), 2007, 9(1): [6],,,. [J]., 2007, 17(7): Chen JJ, Yang SX, Yang QR, et al. Progress in study on effects of aluminum on human health and food safety [J]. Chin J Health Lab Technol, 2007, 17(7): [7]. [J] , 6(5): Pang J. Progress in study on aluminum toxicity to the human body and the related food safety [J]. Internal medicine. 2011, 6(5): [8],,. [J]., 2011, 4(21): Qiu LX, Xu FF, Wang LN. A comparison of different preparation approaches for aluminum determination in food [J]. Chin J Health Lab Technol, 2011, 4(21): [9] SC/T [S]. SC/T Salted jellyfish and salted jellyfish head [S]. [10] GB/T [S]. GB/T Determination of aluminum in foods-inductively coupled plasma mass spectrometry [S]. [11],,,. [J]., 2008, 29(9): Cen JW, Li LH, Yang XQ, et al. Determination of alum in jellyfish products by titration method after acid boiling [J]. Food Sci, 2008, 29(9): [12] GB/T [S]. GB/T Determination of aluminum in flour products [S]. [13],,,. [J]., 2007, 29 (12): Zhang ZS, Gao F, Yan J, et al. Study method of determination of

7 4, : 1203 aluminum in aquatic products by Graphite furnace atomic absorption spectrometry [J]. Anal Lab, 2007, 29 (12): [14],,,. ( ) 4 [J]., 2010, 6(3): Cen JW, Li LH, Yang XQ, et al. Comparison of 4 determination methods of alum(aluminum) in jellyfish [J]. South China Fish Sci, 2010, 6(3): [15],,. [J]., 2010, 27(3): Chen C, Song YH, Gao XQ. Dry and wet digestion determination of aluminum content in Laver [J]. J Food Safe Qual, 2010, 27(3): [16] Sun M, Wu Q. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite atomic absorption spectrometry [J]. J Hazard Mater, 2010, 176(1 3): [17] Ramachandraiah C, Rajesh KJ, Reddys A, et al. Development of a highly sensitive and selective for extractive spectrophotometric determination of aluminum(iii)from environmental matrices synthetic mixtures, and alloys using orthohydroxy propiophenonei sonicotinoylhydrazone [J]. Environ Monit Assess, 2010, 160 (1 4): [18] Ziola-frankowska A, Frankowski M, Siepeak J. Development of a new analytical method for online simultaneous qualitative determination of aluminum (free aluminum ion, alumium- fluoride complexes) by HPLC-FAAS[J]. Talanta, 2009, 78(2): [19] Al-Kindy SMZ, Al-Ghamari SS, Suliman FEO. A sequential injection method for the fluorimetric determination of aluminium in drinking water using 5-quinoline salfonic acid[j]. Spectrochem Acta Part A, 2007, 68: [20] Saiyed SM, Yokel RA. Aluminium content of some foods and products in the USA, with aluminum food additives[j]. Food Addit Contam, 2005, 22(3): 作者简介 ( 责任编辑 : 赵静 ) 白艳艳, 助理研究员, 主要方向为水产品质量安全 [email protected] 张秀珍, 研究员, 主要方向为水产品质量安全检测与标准化 zxz @126.com

Microsoft Word - 4839-4843 20150924002-李建煌-二校全出

Microsoft Word - 4839-4843 20150924002-李建煌-二校全出 6 12 Vol. 6 No. 12 215 12 Journal of Food Safety and Quality Dec., 215 ONPG 李建煌 1, 姚蕾 1, 李玉优 1, 李焕仪 1, 何亮辉 1, 姜春宝 2, 曹维强 (1., 51852; 2., 5166) 1* 摘要 : 目的 βd(onitrophenylβdgalactopyranoside,