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1 3 5 Vol. 3 No Journal of Food Safety and Quality Oct., 2012 吴小娟, 蔡健荣 *, 韩恩, 周立娜, 陈铭枫 (, ) 摘要 : 目的方法,, 结果, ph,,, V, 5~100 μg/l(r=0.9965), μg/l 结论关键词 : ; ; ; ; Determination of trace lead in honey with in-situ bismuth film electrode by square wave stripping voltammetry WU Xiao-Juan, CAI Jian-Rong *, HAN En, ZHOU Li-Na, CHEN Ming-Feng (School of Food and Biological Engineering, Jiangsu University, Zhenjiang , China) ABSTRACT: Objective To determine the trace lead in honey with in-situ bismuth film electrode by square wave stripping voltammetry. Methods Using glassycarbon electrode in-situ plated in bismuth (III), replacing in traditional mercury(ii), the trace lead in honey was rapidly detected by square wave stripping voltammetry method. Results Several factors were optimized, including buffer solutions, ph, the concentration of Bi 3+, plating potential and plating time. Sensitive stripping peak of lead was obtained at the potential of V in the bismuth film electrode. Under the optimized analytical condition, the stripping peak currents were changed linearly with the concentration of Pb 2+ over range from 5 ~100 μg/l (r=0.9965) with a detection limit of μg/l. The result was in accordance with that of graphite furnace atomic absorption spectrometry (GFAAS). Conclusion The established method is rapid and accurate in detecting trace lead in honey. KEY WORDS: electrochemistry; in-situ plating bismuth film; stripping voltammetry; lead; honey,,, [1], ICP [2-5],,,,,,, 基金项目 ( ) * 通讯作者 :,,, Jrcai@ujs.edu.cn

Ming-Feng (School of Food and Biological Engineering, Jiangsu University, Zhenjiang 212013, China) ABSTRACT: Objective To determine the trace lead in honey with in-situ bismuth film electrode by

2 458 3 [6-8] 2000, Wang [9],,,, [10-11],,,, [12], [13], 1 mg/kg,,, 1 实验部分 1.1 主要仪器和试剂 CHI660D ( ); AA240GTA120 ( ); MDS-2002A ( ) : g (, ), 100 ml, 1 g/l Pb mg/l Pb 2+ Bi 3+ : g (, ), 250 ml, 100 mg/l Bi 3+ 5 mg/l Bi 3+ Hg 2+ : g (, ), 100 ml, 1 g/l Hg 2+ 5 mg/l Hg 2+, (,, ) (1 5),,, 1.2 电化学检测 ( 3 mm),,, μm Al 2 O 3 ; 1 mol/l 5 min Bi 3+ Pb 2+,, 0.9 V 180 s,, 30 s,, : 0.9~0 V, : V, : V, : 15 Hz, 样品预处理 0.5 g,, 6 ml, 180,,, 2 ml 1 ml,, min,, 25 ml 1.4 石墨炉原子吸收光谱法检测 GB : nm, 0.2~1.0 nm, 5~7 ma, 120, 20 s; 450, 15~20 s, 1700~2300, 4~5 s, 2 结果与讨论 2.1 检测条件的优化电极的选择 0.2 mol/l ph 4.5, 50 μg/l, Pb 2+,,, Bi 3+ Hg μg/l, Pb 2+, 支持电解质的选择 0.1 mol/l HCl, 0.1 mol/l KCl, 0.1 mol/l (ph=4.5), 0.1 mol/l (ph=4.5) 0.2 mol/l (ph=4.5), 50 μg/l, 400 μg/l Bi mol/l (ph=4.5),, ph 的选择 Bi 3+,

05 μm Al 2 O 3 ; 1 mol/l 5 min Bi 3+ Pb 2+,, 0.9 V 180 s,, 30 s,, : 0.9~0 V, : 0.005 V, : 0.025 V, : 15 Hz, 25 1.3 样品预处理 0.5 g,, 6 ml, 180,,, 2 ml 1 ml,, 180 30 min,, 25 ml 1.

3 5, : mol/l, 50 μg/l, Bi μg/l, ph 3~6, 1, ph 3~5,,, ph, ph=5 3,, 0.9 V, Fig. 3 3 Effects of plating potential on the peak current 1 ph Fig.1 Effects of ph on the peak current 铋浓度的选择 50 μg/l, Bi 3+ 0~600 μg/l, 2, Bi 3+ 0~200 μg/l,, Bi 3+,,, 200 μg/l 沉积时间的选择 4 (0~600 s),,,, 180 s Fig. 4 4 Effects of plating time on the peak current 2.2 工作曲线 2 Bi 3+ Fig. 2 Effects of the concentration of Bi 3+ on the peak current 沉积电位的选择 1.3~ 0.7 V,, 5~100 μg/l Pb 2+ Pb 2+ : Y (μa)=0.3483x (μg/l) (r=0.9965) IUPAC : L= μg/l(n=21)

1.6 沉积时间的选择 4 (0~600 s),,,, 180 s Fig. 4 4 Effects of plating time on the peak current 2.2 工作曲线 2 Bi 3+ Fig.

4 干扰实验 50 μg/l Pb 2+, 5%, : Fe 3+ (100 ) Cl - (300 ) K + (200 ) Na + (100 ) CrO 2-4 (100 )(n=5) 2.4 样品测定与回收率实验 5 Pb 2+ Fig. 5 Standard curve of lead ion ,, 1 GFAAS t, n 1=2, =0.05, t 4.303, t 2.000, t <t(, f), Table 1 表 1 蜂蜜样品中铅的测定和回收率 (n=3) Determination of lead and the recovery in honey samples(n=3) (μg/g) (μg/g) RSD (%) GFAAS (μg/g) (μg/g) (μg/g) (%) ± ± ± 结论,,,,,,,,,,,, 参考文献 [1],. [J]., 2006, 18(5): [2] Duran C, Gundogdu A, Bulut VN, et al. Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)[J]. J Hazard Mater, 2007, 146(1 2): [3] Pohl P. Determination of metal content in honey by atomic absorption and emission spectrometries[j]. Trends Anal Chem, 2009, 28(1): [4] Ioannidou MD, Zachariadis GA, Anthemidis AN, et al. Direct determination of toxic trace metals in honey and sugars using inductively coupled plasma atomic emission spectrometry[j]. Talanta, 2005, 65(1): [5] Zhu ZL, Liu JX, Zhang SC, et al. Determination of Se, Pb, and Sb by atomic fluorescence spectrometry using a new flameless, dielectric barrier discharge atomizer[j]. Spectroch Acta Part B, 2008, 63(3): [6] Sanna G, Pilo MI, Piua PC, et al. Determination of heavy metals in honey by anodic stripping voltammetry at microelectrodes[j]. Anal Chim Acta, 2000, 415(1 2): [7] Li YH, Liu XY, Zeng XD, et al. Simultaneous determination of ultra-trace lead and cadmium at a hydroxyapatite-modified carbon ionic liquid electrode by square-wave stripping voltammetry[j]. Sensor Actuat B Chem 2009, 139(2): [8] Babkina SS, Ulakhovich NN. Amperometric biosensor based on denatured DNA for the study of heavy metals complexing with DNA and their determination in biological, water and food samples[j]. Bioelectrochemistry, 2004, 63(1 2): [9] Wang J, Lu JM, Hocevar SB, et al. Bismuth-Coated Carbon Electrodes for Anodic Stripping Voltammetry[J]. Anal Chem,

000, t <t(, f), Table 1 表 1 蜂蜜样品中铅的测定和回收率 (n=3) Determination of lead and the recovery in honey samples(n=3) (μg/g) (μg/g) RSD (%) GFAAS (μg/g) (μg/g) (μg/g) (%) 0.188 0.172 0.185 0.264 0.

5 5, : , 72(14): 作者简介 [10],,,. [J]., 2008, 36(2): [11],,. [J]., 2002, 30(9): [12] Alghamdi AH. Applications of stripping voltammetric techniques in food analysis[j]. Arab J Chem, 2010, 3 (1) : 1 7. [13] GB , [S]. ( 责任编辑 : 张宏梁 ) 吴小娟,,,, xiaojuan_wu@sina.cn 蔡健荣, 男, 教授, 博士生导师, 主要从事农产品无损检测技术收获机器人技术研究 jrcai@ujs.edu.cn ˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆˇˆ,, , 2012,,,,,,, 2013,, tougao@chinafoodj.com

cn 蔡健荣, 男, 教授, 博士生导师, 主要从事农产品无损检测技术收获机器人技术研究 E-mail: jrcai@ujs.edu.

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<4D6963726F736F667420576F7264202D2033A1A25F484A203737372D323031355FBFD5C6F8BACDB7CFC6F820BFC5C1A3CEEFD6D0BDF0CAF4D4AACBD8B5C4B2E2B6A820B5E7B8D0F1EEBACFB5C8C0EBD7D3CCE5B7A2C9E4B9E2C6D7B7A82E646F63> 中华人民共和国国家环境保护标准 HJ 777-2015 空气和废气颗粒物中金属元素的测定电感耦合等离子体发射光谱法 Ambient air and waste gas from stationary sources emission -Determination of metal elements in ambient