5 3 Vol. 5 No. 3 2014 3 Journal of Food Safety and Quality Mar., 2014 1, 李肖菁 2, 刘丽萍 3, 岳兵 2, 李筱薇 2*, 赵云峰 2, 吴永宁 (1., 430023; 2., 100022; 3., 100013) 1, 2 摘要 : 目的 2013 10, 方法 Z 结果 Z <1, 结论 关键词 : ; ; ; ; Application of quality control graph and international intercalibration study on trace elements in foods in quality control LI Xiao-Jing 1, 2, LIU Li-Ping 2, YUE Bing 2, LI Xiao-Wei 2*, ZHAO Yun-Feng 2, WU Yong-Ning 1, 2 (1. College of Food Technology and Engineering, Wuhan Polytechnic University, Wuhan 300457, China; 2. Key Laboratory for Food Safety Risk Assessment, MOH, China National Centre for Food Safety Risk Assessment, Beijing 100022, China; 3. Central Laboratory of Beijing Center for Disease Control and Prevention, Beijing 100013, China) ABSTRACT: Objectives To explore the application of the quality control graph of the determination of standard reference material and international intercalibration study in quality control by the analysis of our laboratory s results from interlaboratory comparison with trace elements in foods in October 2013. Methods Z-scores were used to appraise the results from the interlaboratory comparison with trace elements in foods organized by International Atomic Energy Agency, and analyzed the determination of the concentrations of trace elements in foods. Results The absolute values of Z-score of concentrations of almost trace elements determined by our laboratory were less than 1, indicating results were excellent. Conclusion The quality control graph and international intercalibration study is a greatly effectively approach of quality control. KEY WORDS: quality control graph; international intercalibration study; food; trace elements; quality control 基金项目 : (2011DFA31770) Fund: Supported by Food Contamination Monitoring and Risk Assessment Techniques Collaborative Research (2011DFA31770) * 通讯作者 :,, E-mail: lixw@cfsa.net.cn *Corresponding author: LI Xiao-Wei, Associate Researcher, China National Center for Food Safety Risk Assessment, No.37, Guangqu Road, Chaoyang District, Beijing 100021, China. E-mail: lixw@cfsa.net.cn
986 5 1 引言,, [1] (inductively coupled plasma mass spectrometry, ICP-MS) ICP-MS ;, ; 7~9 [2] 20 80, 1 ICP-MS, ICP-MS, ICP-MS [3], ICP-MS,,,,, 2~4,, 2 材料与方法 2.1 参加比对实验研究概况, (International Atomic Energy Agency, IAEA) IAEA, [4,5] 2013 10 IAEA-461, 13, 1 表 1 国际实验室比对研究食品样品中多元素含量 Table 1 Concentration of trace elements in food sample from international study on interlaboratory intercalibration (mg/kg) IAEA (mg/kg) Z Cd 0.563 0.571 0.01 Co 4.68 4.84 0.3 Cr 25.8 27.1 0.4 Cu 24.9 26.1 0.4 Fe 2565 2617 0.2 Hg 0.372 0.391 0.4 Mg 6539 6462 0.1 Mn 338 334 0.1 Ni 112 109 0.2 Pb 28.8 26.5 0.7 Se 2.2 2.75 1.6 V 6.38 6.99 0.7 Zn 155 157 0.1 2.2 试剂与仪器 2.2.1 试剂与标准参考物 NIST 1566b, (BVⅢ ),, ( 99.99%), ( 99.999%) : Cd Co Cr Cu Hg
3, : 987 Mn Ni Pb Se Zn 10 mg/l, V 100 mg/l, Fe Mg 1000 mg/l, Agilent, 3% : Li Y Ce Ti Co 10 ng/ml, Agilent : 6 Li Sc Ge Rh Y In Tb Bi 10 μg/ml, Agilent 2.2.2 仪器 ICP-MS: Agilent, 7700 : CEM, MARS 5.0 Milli-Q 2.2.3 仪器分析条件 ICP-MS 2 2.3 测定方法 2.3.1 样品前处理 0.6 g NIST 1566b( 0.001 g) 50 ml 6 ml,,,,, 25 ml 2.3.2 测定 0.1 0.5 1 5 10 50 100 μg/l; 1 5 10 50 100 500 1000 μg/l; 10 50 100 500 1000 5000 10000 μg/l( 3% ), Mass Hunter( Agilent ),,, 2.4 质量控制图的绘制 [1,6] ICP-MS,,, (National Institute of Standards and Technology, NIST) 2.5 比对结果评价方法 Z, Z : (x X ) Z = σ, x= ; X =IAEA ; σ=12.5% [3, 4] 3 结果,, ( ) 1, NIST, 2s -2s, Table 2 表 2 仪器分析条件 ICP-MS instrument operating conditions 1550 W 2 7.0 mm 0.77 L/min 0.1 r/s 0 L/min 0.3 r/s Barbinton 3 1.0 mm, / 1 0.4 mm,
988 5 1 Fig. 1 The quality control graphs of Cd, Co, Fe, Ni, V and Zn 表 3 NIST 1566b 中部分元素含量 Table 3 Concentration of trace elements and in NIST 1566b (mg/kg) Cd 2.48±0.08 Co 0.371±0.009 Fe 205.8±6.8 Ni 1.04±0.09 V 0.577±0.023 Zn 1 424±46 1, NIST 1566b 10,, ;,, 2013 10, 13, 1 Z 1 2 1, mg/kg,,, Z,
3, : 989 Fig. 2 2 Z Z-scores of concentrations of trace elements in food samples : Z -1~1 ; Z 1~2 ; Z 2~3, Z 3 [5,7] 1, Se, 12 4 讨论 1566b,,, 2~3,, 1566b,,,,,,,,, Z <2, 95%, 2< Z <3, 5%, Z >3, 0.1% [3, 7],,,,,, ( ),,,,
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