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1 6 3 Vol. 6 No Journal of Food Safety and Quality Mar., 2015 曾海英 1, 王家磊 1, 沈萍萍 1, 赵玉梅 1, 李钰金 2, 刘远平 3, 毕志明 4, 刘志敏 (1., ; 2., ; 3., ; 4., ) 1* 摘要 : 目的 -ICP-MS 33, 方法 - ICP-MS 7, He, 结果 0.005~0.5 μg/l, RSD 0.58%~4.96%, 81.6%~109%, 结论,,, 关键词 : ; ; ; Determination of 33 kinds of metallic elements in food aquatic products and animal tissues by microwave digestion and ICP-MS method ZENG Hai-Ying 1, WANG Jia-Lei 1, SHEN Ping-Ping 1, ZHAO Yu-Mei 1, LI Yu-Jin 2, LIU Yuan-Ping 3, BI Zhi-Ming 4, LIU Zhi-Min 1* (1. Weihai Shijin Food Inspection Service Co., Ltd., Rongcheng , China; 2. Shandong Provincial Key Laboratory of Processing Techology of Frozen Prepared Food (Taixiang Group), Rongcheng , China; 3. Rongcheng Tai Xiang Food Co., Ltd. (Taixiang group), Rongcheng , China; 4. Rongcheng Food Industry Promotion Agency, Rongcheng , China) ABSTRACT: Objective To establish a method for determination of 33 kinds of elements in food by microwave digestion-icp-ms and internal standard method. Methods The samples firstly was digested, acid-driven and volume controlled by nitric acid-hydrogen peroxide via microwave, and then be tested by the method of ICP-MS. Seven elements were selected as internal standard, which had a good compensation for the analysis of the signal background and the matrix effect. Furthermore, Helium was used as collision-reaction gas, which could effectively get rid of the disturbance of multi-atomic ion. Results The detection limit for each element was 0.005~0.5 g/l, the relative standard deviation (RSD) was 0.58%~4.96%, and the addition standard recovery was 81.6%~109%. The analysis result of the scallop powder elements was in accordance with the given standard. Conclusion The method is of convenience, high sensitivity and good reproducibility and it is 基金项目 : (2012BAD28B05) Fund: Supported by the Twelve Five National Science and Technology Support Project (2012BAD28B05) * 通讯作者 :,,, xndlzm@163.com *Corresponding author: LIU Zhi-Min, Engineer, Weihai Shijin Food Inspection Service Co., Ltd., the 7th of Eshishan Road, Shidao Managing Zone, Rongcheng City, Rongcheng , China. xndlzm@163.com

2 954 6 a reliable and efficient method for the analysis of multi-elements in food samples. KEY WORDS: microwave digestion; inductively coupled plasma mass spectrometry; heavy metals; food safety 1 引言,,,,,, WTO,,,, [1-5],, [6-8],,,,,,, [7-10], ;,, [11-13],,,, [14-17] ICP,,, [18-20],,, 2 材料与方法 2.1 材料与试剂 ( ); ( ) 65% (, ); 30% (, ); Li Sc Ge Y In Tb Bi (100 mg/l, Agilent.U.S.A); 27 (10 mg/l, Agilent.U.S.A); (10 mg/l, Agilent U.S.A); B Ti Mo Sn Sb(1000 mg/l, ); ( %); ( %); (1.0 ng/ml 7 Li, 89 Y, 140 Ce and 205 TI, Agilent U.S.A) 2.2 仪器与设备 (AR1140, ); (MARS Xpress, CEM ); (, CEM); (GM-200, ); (DGL-2001A, ); (KQ-500DE, ); (Angilent7700X, Agilent ) 2.3 实验方法样品的前处理方法 (1),,, 500 g,,,,, (1+4) 24 h,, (2), 0.5~0.7 g( g), 0.4~0.5 g( g), 0.2~0.3 g( g), 5 ml,,, 1 h, 1 ml,,,,, 1, 2 h,,, ;,

3 3, : -ICP-MS , 50 ml,,, 仪器条件样品测定 (1) mg/l, 0.1 mg/l, 3 (2), ICP-MS, 3,, 10%,,, 方法检出限, 11, σ, µg /L, R 0.995, K, Table 1 表 1 微波消解参考条件 Reference conditions of microwave digestion / % : / : : :00 180~190 15:00 表 2 ICP-MS 仪器条件 Table 2 ICP-MS instrument conditions Agilent 7700X ICP-MS Babbington Piltier 2±0.1, 2.5 mm Ni 1550 W 7.5 mm 1.05 L/min Li6 Sc Ge Y In Tb Bi=1.0 mg/l 1.0 ng/ml 7 Li 89 Y 140 Ce 205 TI 89 Y>4000, 140 Ce> TI>1000 CeO/Ce<1.5% Ce 2+ /Ce<3.0% : Ge(72) ; Bi(209) , Table 3 表 3 混合标准溶液中各元素浓度 Each element of mixed standard solution concentration (μg/l) (μg/l) :

4 D L (ng) K : K ; 11 ; : μg/kg 0.05 μg/kg 0.05 μg/kg μg/kg 0.1 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.5 μg/kg 0.1 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.5 μg/kg 0.5 μg/kg 0.5 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.1 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.05 μg/kg 0.1 μg/kg 0.05 μg/kg 0.1 μg/kg 3 结果与讨论 3.1 微波消解条件的确定,,,,,,,,, ;,,, 1,,,,, 4 1, 5 ml, 5 ml 1 ml, 5 ml 1 ml 1 ml,, 5, 5 ml, 5 5 ml +1 ml,,,, 5 ml +1 ml 3.2 方法的确认添加回收率方法精密度标准曲线线性回归方程和相关系数,,,,, 6, 6, 81.6%~109%, RSD 0.58%~4.96%, R 0.996, 表 4 微波消解法与国家标准中湿法消解的比较 Table 4 Comparison of microwave digestion and wet digestion (%) (%) Table 5 表 5 不同消解溶液消解效果的比较 The comparison of different digestion solution dissolve 5 ml 5 ml +1 ml 5 ml +1 ml +1 ml

5 3, : -ICP-MS Table 6 表 6 添加回收率相对偏差及线性关系 Spiked recoveries, relative standard deviations and linear relationships (μg/l) (%) RSD(%) R Li Be V Cr Mn Co Ni Cu Zn Ga As Se Y=0.0051X Y=0.0024X Y=0.0024X Y=0.0022X Y=0.0305X Y=0.0257X E Y=0.0046X E Y=0.0758X Y=0.0202X Y=0.1205X Y=0.0187X E Y=0.0016X E

6 958 6 (μg/l) (%) RSD(%) R 续表 6 Rb Sr U Ag Cd Cs Ba Hg Tl Pb Na Mg Y=0.1423X Y=0.0253X Y=0.0218X Y=0.0086X Y=0.0021X Y=0.0024X Y=0.0023X Y=8.5437E-004X Y=0.0190X Y=0.0239X Y= X Y=5.0954X

7 3, : -ICP-MS (μg/l) (%) RSD(%) R 续表 6 K Ca Fe Y=5.7240X Y=0.0192X Y= X Table 7 表 7 标准物质测定值与标准值比对表 Comparison of standard material measured value and standard value (μg/kg) (μg/kg) (μg/kg) (μg/kg) ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ICP-MS 仪器条件的选择及干扰的消除,, He,,, ( ),,, ( ),, ; Li Sc Ge Y In Tb Bi, 3.3 方法的精确度,,, 7 7

8 结论 ICP-MS Hg As Pb Cd Sn Se Zn Al Sb Fe Cr Mn Cu Ti Ni Na Mg Ca Li Be V Mn Co U Rb Sr Ag Cs Mo B Ba Tl K33, ICP-MS : (1) 5 ml +1 ml ; (2), He,,, 参考文献 [1],,,. ICP-MS [C]., 2007, Wang CL,Zhang P,Qi JY, et al. Microwave digestion ICP-MS determination of trace heavy metal elements in rice [C]. Proceedings of the fourth national conference on environmental chemistry academic, 2007, [2]. ICP-MS 12 [J]., 2012, 28(5): Yuan J. Determination of 12 Metals in Soil and Sediment by Microwave Digestion and ICP-MS [J]. Environ Mon China, 2012, 28(5): [3],. [J]., 2006, 27(3): 184. Song JE, Yu S. Application of inductively coupled plasma mass spectrometry in clinical samples analysis [J]. J Chin Mass Spect Soc, 2006, 27(3): 184. [4],,,. ICP-MS AFS GF-AAS As Cd Hg Pb [J]. 2009, (04): Chen GY, Du YQ, Li W, et al. Method comparison to determination of As Cd Hg Pb in food by ICP-MS AFS GF-AAS [J]. J Chin Mass Spect Soc, 2009, (04): [5],,,. ICP-MS GFAAS [J]., 2011, 01: Pang YH, Xiao SS, Sun XQ, et al. Comparison between ICP-MS and GFAAS for determination of lead and codmium in alga food [J]. Chin J Spect Lab, 2011, 01: [6],,. ICP-MS [J]., 2009, 04(34): Lu WM, Zhang J, Gong WD. Method for analysis of several elements in surface water by ICP-MS [J]. Environ Sci Manag, 2009, 04(34): [7]. ICP-MS [J]., 2012, 06: Xu XL. Determination of heavy metal elements in lentinus edodes by microwave digestion and inductively coupled mass spectromentry [J]. Edible Fungi China, 2012, 06: [8],,. 16 [J]., 2010, 11: Yang RC, Zhai ZL, Hao DQ. Determ ination for 16 rare- earth elements in root-vagetableby ICP-MS [J]. Chin J Health Lab Technol, 2010, 11: [9],,,. ICP-MS 35 [J]., 2012, 06: Zhang QH, Liao CX, Lin SX, et al. Determination of 35 elements in tea by ICP-MS after microwave digestion [J]. Guizhou Sci, 2012, 06: [10],,,. ICP-MS [J]., 2013, 6: Huang XC, Liu CH, Zhang J, et al. Two microwave digestion pretreatment methods for determination of heavy metal in vegetable samples [J]. Rock Min Anal, 2013, 6: [11] Elzbieta (Ela) Bakbwska. ICP-MS EPA200.8 [J]., 2001,06: Elzbieta (Ela) Bakbwska. Application of icp-ms technology and EPA200.8 standard method analysis of drinking water and wastewater samples [J]. J Environ Chem, 2001, 06: [12] EPA Method Determination of trace elements in waters and wastes by inductively coupled plasma-mass spectrometry[s]. [13],,. ICP-MS [C]., 2003: Xu T, Hao DM, Zhang YM. Microwave digestion icp-ms method for determination of copper, lead, arsenic, tin in food [C]. Volume of the 10th national rare earth elements in analytical chemistry academic report, 2003: [14],,. Pb As

9 3, : -ICP-MS [J]., 2001, 02, 23(2): Wu XZ, Tang YJ, He GZ. Microwave digestion was developed for the determination of metallic elements such As Pb, As in food method [J]. J Ningxia Med J, 2001, 2, 23(2): [15],,,. [J]., 2007, (2): Fang YM, Lu G, Xiong LB, et al. The microwave digestion of lead, cadmium, arsenic and mercury in the food of the method [J]. J Environ Occup Med, 2007, (2): [16],,. ICP-MS [J]., 1999, 19(4): Sun YL, Chen MS, Wang YP, et al. Microwave acid-digestion ICP-MS method for the determination of sixteen elements in marine products [J]. Spect Spect Anal, 1999, 19(4): [17],,,. ICP-MS [J]., 2002, 29(1): Liu F, Dai JJ, Lin YZ, et al. ICP-MS determination of metal elements in food [J]. Mod Prev Med, 2002, 29(1): [18],,,. /ICP-MS 9 [J]., 2012, 32(3): Liang SY, Wang X, Wu H, et al. Determination of 9 heavy metal elements in sediment by ICP-MS using microwave digestion for sample preparation [J]. Spect Spect Anal, 2012, 32(3): [19]. ICP-MS 14 [J]., 2007, 26(5): Chen GY. Simultaneous determination of 14 elements in vegetables by ICP-MS with microwave digestion [J]. J Instrum Anal, 2007, 26(5): [20]. [M]. :, Wang XR. Inductively coupled plasma mass spectrometry application examples [M]. Beijing: Chemical Industry Press, 作者简介 ( 责任编辑 : 杨翠娜 ) 曾海英, 本科, 中级职称, 主要研究方向为元素检测 @qq.com 刘志敏, 硕士研究生, 中级职称, 主要研究方向为食品检测 xndlzm@163.com

Microsoft Word 张遴-二校

Microsoft Word 张遴-二校 6 2 Vol. 6 No. 2 2015 2 Journal of Food Safety and Quality Feb., 2015 张遴 1*, 钟战强 1, 乔冠华 1, 邓阿粉 2 (1., 710068; 2., 710068) 摘要 : 目的方法,, 结果, 0.999, 0.03 μg/kg 0.12 μg/kg, (RSD) 3.5% 8.1%, 96% 116% 结论, 关键词