Microsoft Word 蔡文华-二校 3337.doc

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1 5 10 Vol. 5 No Journal of Food Safety and Quality Oct., 2014 蔡文华 1*, 苏祖俭 1, 胡曙光 1, 黄伟雄 1, 姚敬 1, 张学武 1, 钟杰伟 2, 李元尊 (1., ; 2., ; 3., ) 3 摘要 : 目的, 方法, 结果 (LOQ) 0.06 μg/l 0.15 μg/l; (r) , RSD 4.9% 4.1%; GBW10048-, ; 6, GBW GBW10043-, 结论, 关键词 : ; ; Study on quality control of the determination of mercury in food safety risk monitoring CAI Wen-Hua 1*, SU Zu-Jian 1, HU Shu-Guang 1, HUANG Wei-Xiong 1, YAO Jing 1, ZHANG Xue-Wu 1, ZHONG Jie-Wei 2, LI Yuan-Zun 3 (1. Reference Laboratory of Heavy Metals of National Food Safety Risk Monitoring, Center for Disease Control and Prevention of Guangdong Province, Guangzhou , China; 2. Center for Disease Control and Prevention of Zhanjiang City, Zhanjiang , China; 3. Center for Disease Control and Prevention of Maoming City, Maoming , China) ABSTRACT: Objective To improve the accuracy of experimental results by means of quality control of the determination of mercury in food. Methods A comparison was made after the determination of mercury in multiple standard substance with different pretreatment and assay methods. The difference in the storage conditions of determination results of mercury was also found. Results The LOQs of mercury determined by ICP-MS and AFS were 0.06 μg/l and 0.15 μg/l, respectively. The correlation coefficients were both The RSDs were 4.9% and 4.1%, respectively. The results of GBW10048 with three pretreatment methods were found to be within tolerable limits. However, the results made by microwave digestion and high pressure digestion had a better precision. The results of 6 kinds of standard substances determined by ICP-MS were all in the scope of standard values. While, the results determined by AFS were also in the scope of standard values except GBW10018 and GBW10043 with low mercury contents. Conclusion It will contribute to advance the accuracy of trace mercury determinations via strict quality control and appropriate measure. KEY WORDS: mercury; trace analysis; quality control * 通讯作者 :,, yisacai_1@126.com *Corresponding author: CAI Wen-Hua, Technologist-in-Charge, Center for Disease Control and Prevention of Guangdong Province, No. 160, Qunxian Road, Dashi District, Guangzhou , China. yisacai_1@126.com

2 引言 (mercury),,, [1,2], [3,4],, : (, 10 μg/kg);, ;,, ;,,, 2000~2014,, 2 材料与方法 2.1 仪器与试剂主要仪器 AFS-9130 (); Agilent 7700x (ICP-MS, ); MWS-2 ( Berghof); AED-440 ( ); LabTech-EH20B (); 50 ml ; 主要试剂 ( Merck KGaA); : , (1%) 1.0 mg/l 115 In 209 Bi ( ); : , (1%) 10 μg/l 7 Li 39 Co 89 Y 140 Ce 205 Tl ( ) >18.2 MΩ cm 标准溶液及标准物质 : GSB G , 1000 mg/l, ; : (5%) 2.0 μg/l; GBW08508( ); GBW10014( ); GBW10024( ); GBW10018( ); GBW10043( ); GBW10050( ); GBW10048( ) 2.2 实验方法试样预处理 (1),, 20,,,, (2),,,, 试样前处理 (1) 0.5~3 g( 0.1 mg) 50 ml, 8 ml HNO 3, h, 160 6h,,,, 20 ml, (2) 0.2~0.5 g, 0.5~1.0 g( 0.1 mg), 5 ml HNO 3 25~ min; 145~ min; 160~ min, 120~140 15~30 min,,, 20 ml, (3) 0.5~2 g( 0.1 mg), 5 ml HNO ~6 h,, 120~140 15~30 min,,, 20 ml, 测定方法 (1) 原子荧光 (AFS) 测定汞,

3 10, : %-, 5%, 270 V, 30 A, 10 mm, 400 ml/min, 800 ml/min 0~2.0 µg /L5 (2) 电感耦合等离子体质谱法 (ICP-MS) 测定汞 (, ),, 0~2.0 µg /L, 5 3 结果及讨论 3.1 实验环境及试剂的质量控制, 20%,, 50% -, 100~250 μg/l 3.2 容器吸附汞的质量控制, 1,,,, ; 20% (0.5 g/l) (5%),,,,,,,, 5%, [5], 1 d 3.3 检出限和精密度, (AFS) (ICP-MS), 1,,, 1 Fig.1 ( - : μg/l) Three concentrations of mercury in various storage conditions with time in attenuation. (From left to right mercury concentrations were: μg/l)

4 Table 1 表 1 检出限和精密度 Thedetection limits and precision LOD n=21 LOQ n=21 RSD n=7 r μg/l μg/l μg/l % AFS ~ ICP-MS ~ : 0.5 g, 20 ml, AFS (LOQ) 6 μg/kg, ICP-MS (LOQ) 3 μg/kg 3.4 不同前处理方法的比较与质量控制湿法消解, 50 ml : (1), [6,7], ; (2),,,,, 高压罐消解,,, [8,9], : (1), ; (2), ; (3) 微波消解, [10,11] :,, 三种前处理方式测定结果对比 GBW ( 2),, ;,,,, 3.5 不同测定方法的对比与质量控制氢化物发生 - 原子荧光光谱法 :,,, 32, 80, 1 ng ml (n 11); 20, 47, 1 ng ml (n 11) [12], :,,,,,,,, [13] :,, [14], 2%~5% HNO 3, 0.5%- Table 2 表 2 不同前处理方式测定结果对比 (n=7) The comparison of determination results of different pretreatment methods(n=7) (µg/kg) (µg/kg) (µg/kg) RSD(%) ± : ICP-MS

5 10, : 3341 Table 3 表 3 两种方法测定标准物质的测定结果 (n=7) Results of two methods for determination of standardsubstance(n=7) AFS ICP-MS (µg/kg) RSD(%) (µg/kg) RSD(%) (µg/kg) GBW ±1.5 GBW ±0.8 GBW ±1.6 GBW ±3 GBW ±7 GBW ±7 : 电感耦合等离子体质谱法,, 209 Bi,,, 5%, 5%,,,, 100 μg/l, 两种测定方式结果对比 3,, ;,, 4 结论,,,, ;, ;, 参考文献 [1] Manutseween, Aeungmaitrepirom W, Varanusupakul P, et al. Determination of Cd, Cu, and Zn in fish and mussel by AAS after ultrasound-assisted acid leaching extraction[j]. Food Chem, 2007, 101: [2],. [J]., 2001, 16(4): Shuai JS,Wang L. Discussion on effects on human health and countermeasures of heavy metal pollution[j]. Environ Devel, 2001, 16(4): [3] Setting maximum levels for certain contaminants in foodstuffs. Commission regulation (EC) No : European Union, [4] US EPA. What you need to know about mercury in fish and shellfish. New York: US EPA, [5] WHO. Summary and conclusions of the sixty-first meeting of the joint FAO/WHO expert committee on food additives(jecfa), JECFA/61/SC. Geneva: WHO, [6] GB Maximum levels of contaminants in foods[s]. [7],,. ICP-MS [J]., 2009, 7: Xie YX, Li DL, Zuo YX. Research on determination of Hg in drinking water by ICP-MS [J]. Life Sci Instrum, 2009, 7: [8] Mohammad S, Tahir HZ. Several affecting factors in digestion methods on measurement of total mercury in fish[j]. Anal Chem, 1984, 1(3): [9],. [J]., 2007, 24(7): Li J, Zhou LP. Effect of digestion methods on measurement of total mercury in fish by hydride seneration-cold vapor AAS [J]. Stud Trace Elem Heath, 2007, 24(7): [10],. -

6 [J]., 2011,18(5): Liu JC, Li X. Determination of Cu in milk by high pressure digestion-atomic absorption spectrometry [J]. Chin J Health Inspect, 2011, 18(5): [11],,,. - [J]., 2005, 25(8): Shi J, Song QG, Zhao KL et al. Determination of trace bismuth in traditional chinese medicines by hydride generation atomic fluorescence spectrometry[j]. Spectrom Spect Anal, 2005, 25(8): [12],. [J]., 2008, 22(2): Luo YL, Ni HY. Discussion on microwave digestion[j]. Tianjin Chem Ind, 2008, 22(2): [13],. [J]., 2003, 9(4): Liu CP, Fang Y. Microwave digestion technique in the application of element analysis [J]. Anhui J Prevent Med, 2003, 9(4): [14],,,. - - [J]., 2004, 24(2): Mou RX, Chen MX, Zhu ZW et al. Determination of trace mercury in rice by microwave digestion-hydride generation- atomic fluorescence spectrometry[j]. Spectrom Spect Anal, 2004, 24(2): [15],. [M]. :, Chen LP, Zhou SC. Modern chemical experiment and technology [M]. Beijing: Science Press, [16],,. - [J]., 2008, 24(5), Chen J, Pan WC, Guo GH. Determination of mercury in blood by microwave digestion-atomic fluorescence spectrometry [J]. Occup Health, 2008, 24(5): 作者简介 ( 责任编辑 : 杨翠娜 ) 蔡文华, 硕士, 主管技师, 主要研究方向为食品检验与食品安全风险监测 yisacai_1@126.com

Microsoft Word 聂雪梅.doc

Microsoft Word 聂雪梅.doc 4 4 Vol. 4 No. 4 2013 8 Journal of Food Safety and Quality Aug., 2013 聂雪梅 *, 李立, 孙利, 高飞 (, 100123) 摘要 : 2011 12,, 2007~2011,,,, 关键词 : ; ; ; ; Trade and notification situation on food import and export