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1 8 5 Vol. 8 No Journal of Food Safety and Quality May., 韩晓鸥 *, 平小红, 张媛媛 (, ) 摘要 : 目的 - As( Ⅲ) ; 方法 20 ml 0.15 mol/l HNO 3, h, 结果 As( Ⅲ) 7.6%, As( Ⅴ) 3.1% 结论, 关键词 : ; ; ; ; Determination of inorganic arsenic content in seafood by liquid chromatography-atomic fluorescence spectrometry and its risk assessment HAN Xiao-Ou *, PING Xiao-Hong, ZHANG Yuan-Yuan (Liaoning Provincial Center for Disease Control and Prevention, Shenyang , China) ABSTRACT: Objective To establish a method for determination of 2 kinds of inorganic arsenic including arsenite As (Ⅲ) and arsenate As (Ⅴ) in seafood by liquid chromatography-atomic fluorescence spectrometry (LC-AFS), and to establish a mathematical model to infer the probability of inorganic arsenic positive samples in the markets. Methods Samples were soaked in 20 ml 0.15 mol/l HNO 3 solutions over night, and were heat extracted in a thermostat at 90 for 3 h. After being cooled, the extract was introduced for LC-AFS analysis. The mathematical model was established by using the risk assessment Results The prevalence rate of arsenite As (Ⅲ) was 7.6% and the prevalence rate of arsenate As (Ⅴ) was 3.1%. Conclusion The established model can infer the probability of inorganic arsenic positive samples in seafood and water samples in large supermarkets and small markets, which can provide technical support for the risk management of seafood. KEY WORDS: liquid chromatography; atomic fluorescence spectrometry; seafood; inorganic arsenic; risk assessment * 通讯作者 :,,, @qq.com *Corresponding author: HAN Xiao-Ou, Engineer, Liaoning Provincial Center for Disease Control and Prevention, Shenyang , China @qq.com

2 5, : 引言, Omega-3(ω-3) [1],,, [2],,,,,, [3-5] (As),, [As(Ⅲ) As( Ⅴ )], (monomethylarsine, MMA) (dimethylarsine DMA), GB [6], 0.1 mg/kg, 0.5 mg/kg, [As(Ⅲ) As( Ⅴ )], GB [7], - (liquid chromatography-atomic fluorescence spectrometry, LC-AFS) -(liquid chromatography-inductively coupled plasma mass spectrometry, LC-ICP/MS), LC-ICP/MS, [8-14] LC-AFS, [15] 2 材料和方法 2.1 材料与试剂 200, 30, 30, 70, 70, (, ) (, 96%, ); (, 85%, ); (, 65%~68%, ); (, 36%~38%, ); (, 99.9%, ); As(Ⅲ)(GBW 08667, ); As(Ⅴ)(GBW08666, ) 2.2 仪器与设备 e2695 ( ); AFS-9730 (); KQ5200DB ( ); Milli-Q ( Millipore ); ( ); LAB DANCER S25 ( ); BS110S ( ); S25 ( ); ( ml, Eppendorf ); ( ) 2.3 试验方法 标准溶液的配制 As(Ⅲ): μg/g 20 μl, 1.5 ml, 1000 ng/ml As(Ⅴ): 32.4 μg/g 86 μl, 1.5 ml, 1000 ng/ml 仪器条件 : :, Hamilton PRP X-100(250 mm 4.1 mm,10 μm); 30 ; : 5 mmol/l, 45 mmol/l, ph 5.92; 100 μl : 75 ma, 300 V, 400 ml/min, 800 ml/min, 8 mm 线性范围和检出限 : As( Ⅲ) As( Ⅴ) μl 2.0 ml, ng/ml, 100 μl (Y), (X), g, 11, 样品前处理, g( g), 50 ml, 20 ml 0.15 mol/l HNO 3, h, 0.5 h 1 min,, r/min 15 min, 5 ml, 5 ml, 1 min, r/min 15 min, 1,, 0.45 μm 回收率和精密度,, 1000 μg/l ml, 24 h, 2.3.3

3 1928 8, 6, 结果与分析 3.1 线性范围和检出限 1 : 2 1.8, 2 ( 1) 2, g, As( Ⅲ ) mg/kg, mg/kg, As( Ⅴ) mg/kg, mg/kg 3.2 提取条件的选择 提取溶剂 ( ml) As( Ⅲ) As( Ⅴ)2, 2 2, ml, As( Ⅲ),,,, 20 ml 提取温度和时间 As( Ⅲ) 2,, 90, h As( Ⅲ) As( Ⅴ),, 3 h, 3 h 3.3 方法回收率和精密度 2 2, As( Ⅲ) 91.3% 97.5%, (relative standard deviation, RSD) 0.6% 2.8%,, Fig Chromatogram of standard mixture of 2 kinds of inorganic arsenic Table 1 表 1 线性回归方程和相关系数 Regression equations and correlation coefficients (ng/ml) (mg/kg) (mg/kg) As( Ⅲ ) 0 50 Y=0.04X+5.379e As( Ⅴ ) 0 50 Y=0.04X+3.59e

4 5, : As( Ⅲ), RiskTriang (0.06, 0.07, 0.1) 3 Table 3 表 3 样品检测结果 Analytical results of samples ( ) As( Ⅲ) (%) 6.7% 10.0% 5.7% 8.6% 7.5% Fig. 2 As( Ⅲ ) As( Ⅴ ) Table 2 2 Effects of extraction solvent volumes on recoveries 表 2 回收率与精密度 (n=6) Results of precision and recovery (n=6) (ng/ml) 3.4 暴露评估模型建立 (ng/ml) (%) (%) , 3 As( Ⅲ), (0.5 mg/kg) As( Ⅲ) As( Ⅴ), 亚砷酸盐 As( Ⅲ ) 阳性样品流行率模型 3, As( Ⅴ) (%) 3.3% 3.3% 2.9% 2.9% 4.0%, As( Ⅲ) 6.472%~9.206%, As( Ⅲ) 7.6%, As( Ⅲ) 7.6% 超级市场水产品和水产制品中 As( Ⅲ ) 阳性样品预测模型 50, As( Ⅲ) 7.6%, 50 As( Ⅲ) RiskBinomial(50,0.076) 4 As( Ⅲ) 1 3.8% 中小市场水产品和水产制品中 As( Ⅲ ) 阳性样品预测模型 30, 7.6%, 30 As( Ⅲ) RiskBinomial(30,0.076) Fig. 3 3 As( Ⅲ) The prevalence rate of arsenite As(Ⅲ) in Liaoning

5 As( Ⅲ) Fig. 4 The inferior quality of sea food of arsenite As(Ⅲ) in supermarkets Fig. 5 5 As( Ⅲ) The inferior quality of sea food of arsenite As(Ⅲ) in medium and small markets 5 As( Ⅲ) % 水产品和水产制品中 As( Ⅴ ) 阳性样品流行率模型 3, As( Ⅴ), RiskTriang (0.029, 0.031, 0.033) 6, As( Ⅴ) %~3.2331%, As( Ⅴ) 3.1%, As( Ⅲ) 3.1% 大型超级市场水产品和水产制品中 As( Ⅴ ) 阳性样品预测模型 50, As( Ⅴ) 3.1%, 50 As( Ⅴ) RiskBinomial (50,0.031) 7 As( Ⅴ) 1 1.6% 中小市场水产品和水产制品 As( Ⅴ ) 阳性样品预测模型 30, 3.1%, 30 RiskBinomial(30,0.031) 8 As( Ⅲ) %

6 5, : As( Ⅴ) Fig. 6 The prevalence rate of arsenate As( Ⅴ) in Liaoning 7 As( Ⅴ) Fig. 7 The inferior quality of sea food of arsenate As( Ⅴ) in supermarkets 8 As( Ⅴ) Fig. 8 The inferior quality of sea food of arsenate As( Ⅴ ) in medium and small markets

7 结论与讨论, As( Ⅲ) 7.6%, As( Ⅲ) 1 3.8%, As( Ⅲ) % 3.1%, As( Ⅴ) 1 1.6%, % As( Ⅲ), As( Ⅲ), As( Ⅲ),, As( Ⅲ), As( Ⅲ),, As( Ⅲ),, 参考文献 [1], LI Ke,,, [J]., 2016, 5(44): Wang S, Li K, Cui H, et al. Quantitative analysis of total and different species of arsenic in oil of Antarctic krill (Euphausia superba) [J]. Chin J Anal Chem, 2016, 5(44): [2],,,. [J]., 2011, 7(27): Wu J, Yang X, Jiang P. et al. Distribution of arsenic metabolite in liver of rats treated with arsenite and arsenate [J]. Chin J Public Health, 2011, 7(27): [3],,,. [J]., 2006, 22(8): 956. Xu YY, LI X, Liang XF, et al. Study on urinary arsenic metabolites of population with different concentrations of arsenic in drinking water in Inner Mongolia [J]. Chin J Public Health, 2006, 22(8): 956. [4],,,. [J]., 2003, 22: Zhang AH, Hong F, Huang XX, et al. Study on mechanism of carcinogenic effect and genetic damage of arsenism caused by burning coal pollution [J]. Chin J Endemiol, 2003, 22: [5],,,. [J]., 2010, 33(4): Wu J, Jiang P, Wang H, et al. Extracted methods of arsenic speciation in liver of rats treated with sodium arsenite [J]. J Xinjiang Med Univ, 2010, 33(4): [6] GB [S]. GB China food safety national standard for maximum levels of contaminants in foods [S]. [7] GB [S]. GB/T Determination of total arsenic and inorganic-arsenic in foods [S]. [8] Duker AA, Carranza EJM, Hale M. Arsenic geochemistry and health [J]. Environ Int, 2005, 31: [9] Lloyd-Smith M, Wickens J. Mapping the hotspots: DDT-contaminated dumpsites in Australia [J]. Glob Pestic Camp, 2000, 10: 1. [10] Tyrovola K, Nikolaidis NP. Arsenic mobility and stabilization in topsoils [J]. Water Res, 2009, 43: [11],,,. -- [J]., 2014, 28(2): Tian Y, Cai X, Zheng XB, et al. Arsenic speciation analysis in cinnamon by high performance liquid chromatography-hydride generational atomic fluorescence spectrometry [J]. Chem Eng, 2014, 28(2): [12],,,. - 4 [J]., 2013, 5: Cao J, Yu B, Shen S, et al. Analysis of arsenic speciation in aquatic products and environments by HPLX-HG-AFS [J]. Inspect Quarant Sci, 2013, 5: [13] 喆,,,. - [J]., 2016, 7(3): Dong Z, Gao MY, Li MY, et al. Determination of arsenic content and speciation in foods of different matrixes by high performance liquid chromatography-hydride generation atomic fluorescence spectrometry [J]. J Food Saf Qual, 2016, 7(3): [14],. - [J], 2016, 9(32): Zhang K, Yang CX. Comparison of sample pretreatment methods for analysis of arsenic speciation in kelp and laver by liquid chromatograghy-atomic fluorescence spectrometry [J]. J Prev Med Inf, 2016, 9(32): [15],,,. [J]., 2006, 34(6): Chu XJ, Feng LG Zhang Y, et al. Risk assessment of bacillus cereus in pasteurized milk [J]. China Dairy Ind, 2006, 34(6): 作者简介 ( 责任编辑 : 姜姗 ) 韩晓鸥, 硕士, 工程师, 主要研究方向食品安全 @qq.com