5 4 Vol. 5 No. 4 2014 4 Journal of Food Safety and Quality Apr., 2014 1, 白 艳 艳 2, 谷 伟 丽 3 1,, 马 元 庆 2 1,, 孙 珊 2, 魏 潇 1, 张 秀 珍 (1., 264006; 2., 264006; 3., 264006) 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 264006, China; 2. Shandong Provincial Key Laboratory of Restoration for Marine Ecology, Yantai 264006, China; 3. Yantai Shanshui Seafood Co. Ltd, Yantai 264006, 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 :,, E-mail: zxz0535501@126.com *Corresponding author: ZHANG Xiu-Zhen, Professor, Marine Resources and Environment Research Institute of Shandong Province, No.216, Changjiang Road, Yantai 264006, China. E-mail: zxz0535501@126.com
1198 5 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 23374-2009 [10] S [12] [13], SC/T 3210-2001 [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 2.2.1 样 品 前 处 理 方 法, SC/T 3210-2001 [9] 20 g,, 500 ml,,, [11] 0.6 mol/l 6 min, CEM MARS : ~120, 5 min, 120, 5 min; 120~160, 5 min,
4, : 1199 160, 5 min; 160~180, 10 min, 180, 5 min 2~5 g( 0.0001 g), 10 ml,, 140~160, 50 ml, 3,, ;, LabTech EH35B : ~120, 120, 5 min; 180, 180, 2 h, 220 2~5 g( 0.0001 g), 10 ml,,,,,, 10 ml,, 50 ml, 3,, ; 2.2.2 样 品 检 测 方 法,, SC/T 3210-2001 [9] EDTA ICP-MS,, ICP-MS 7500ce 1, 2% 0 10.0 20.0 40.0 80.0 120.0 µg/l 2.3 评 价 方 法 2.3.1 精 密 度 计 算, 2.3.2 回 收 率 试 验 100 200 300 400 500 mg/kg,, 2.3.3 数 据 统 计 方 法 ANOVA Duncan, P<0.01 3 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 3 1300 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,
1200 5 3.2 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 0 65.1 -ICP-MS 0.052 -ICP-MS 62.3 8.60 377 -ICP-MS - 4.12 -ICP-MS - 191 8.17 376 -ICP-MS 8.72 -ICP-MS 384 8.77 400 -ICP-MS 8.82 -ICP-MS 415 163 -ICP-MS 171 561 -ICP-MS 355 562 -ICP-MS 571 577 -ICP-MS 586
4, : 1201 Table 4 表 4 方 法 精 密 度 比 较 Comparison of precision of different determination methods n (mg/kg) RSD% 10 163±10.8 6.59 -ICP-MS 10 171±5.89 3.44 10 561±4.69 0.84 -ICP-MS 10 355±6.81 1.92 10 562±10.6 1.88 -ICP-MS 10 571±6.15 1.08 10 577±9.61 1.67 -ICP-MS 10 586±5.42 0.92 Table 5 表 5 方 法 的 加 标 回 收 率 比 较 Comparison of recoveries of determination methods mg/kg 100 200 300 400 500 -ICP-MS -ICP-MS -ICP-MS -ICP-MS 99.2~100.7 100.7~101.3 101.1~101.5 99.0~101.1 99.9~100.8 101.2 99.7~103.0 99.9~102.2 99.7~104.2 98.9~103.3 99.1~103.1 102.7 92.3~107.8 93.6~105.6 96.2~107.5 95.0~102.2 90.6~109.3 104.4 65.5~81.2 60.2~79.3 70.1~80.1 58.1~80.1 55.1~71.3 78.7 88.8~110.1 92.5~101.5 95.6~111.2 89.9~102.1 90.1~102.3 101.4 89.2~110.3 89.9~101.3 91.3~103.6 99.2~111.3 95.6~105.1 104.9 85.4~111.2 90.2~104.3 89.6~108.2 95.2~107.1 91.2~101.5 105.4 89.3~106.2 90.2~104.2 88.8~110.1 79.6~101.0 80.6~102.1 103.8 3 4 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
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