Microsoft Word 魏茂琼-二校出3673

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1 7 9 Vol. 7 No Journal of Food Safety and Quality Sep., , 魏茂琼 2 1,, 刘宏程 2*, 严红梅 2, 和立忠 2, 王丽 2, 林昕 (1. ( ), ; 2., ) 1, 2 摘要 : 目的 0.3 mol/l 4 ( As III As V MMA DMA) - (liquid chromatography-atomic fluorescence spectrometry, LC-AFS) 方法 60, 40 min, LC-AFS 2 4, 结果 ~0.01 μg/ml, 89.03%~100.70%, RSD 4.36%(n=5) 结论 1 h,, 关键词 : ; ; ; - ; Determination of 4 kinds of arsenic species in rice by liquid chromatographyatomic fluorescence spectrometry WEI Mao-Qiong 1, 2, LIU Hong-Cheng 1, 2*, YAN Hong-Mei 2, HE Li-Zhong 2, WANG Li 2, LIN Xin 1, 2 (1. Laboratory of Quality & Safety Risk Assessment for Agro-Product, Ministry of Agriculture (Kunming), Kunming , China; 2. Agri-Food Quality Standard & Testing Technology Institute, Yunnan Academy of Agricultural Sciences, Kunming , China) ABSTRACT: Objective Using 0.3 mol/l nitric acid as the extractant, to establish a method for the simultaneous determination of arsenious acid (As III), arsenic acid (As V), dimethylarsinic acid (DMA) and monomethylarsinic acid (MMA) in rice by liquid chromatography-atomic fluorescence spectrometry (LC-AFS). Methods After ultrasonic extraction 40 min at 60, the sample was detected by LC-AFS. The extraction efficiency of two kinds of extracted methods was compared. The concentration of nitric acid, extraction temperature and extraction time were optimized. Results The detection limits of 4 kinds of main arsenic species ( As III, As V, DMA, MMA ) in rice were 0.002~0.01 μg/ml, the recoveries were in the range of 89.03%~100.70%, and the relative standard deviations (RSDs) were less than 4.36%(n=5). Conclusion This method can completely separate the 4 kinds of arsenic species in rice samples within 1 h, which is simple, accurate for the risk assessment of heavy metal arsenic in rice. KEY WORDS: rice; arsenic species; ultrasonic extraction; liquid chromatography-atomic fluorescence spectrometry; nitric acid 基金项目 : (2015HC025) ( )(2014DA001) Fund: Supported by the Innovative Team of Yunnan Province (2015HC025) and the Science and Technology Innovation Platform Construction Plan (Public Service of Science and Technology) (2014DA001) * 通讯作者 :,, liuorg@163.com *Corresponding author: LIU Hong-Cheng, Researcher, Laboratory of Quality and Safety Risk Assessment for Agro-products (Kunming), Ministry of Agriculture, Institute of Quality Standards and Testing Technology, Yunnan Academy of Agricultural Sciences, NO.9 Xueyun Road, Kunming , China. liuorg@163.com

2 引言, : (arsenite, As III) (arsenate, As V) (dimethyl arsenic acid, DMA) (monomethyl arsenic acid, MMA) [1] LD 50,, (MMA) (DMA) (AsC), (AsB) [2,3] As V AsC AsB, AsB [4],, [5,6],,,, MMA DMA, [7,8],, [9] - [10] : [11,12] [13] Melgar [14] 晞 [15] - (liquid chromatographyatomic fluorescence spectrometry, LC-AFS), 0.3 mol/l, 4, 样品前处理,, 80, 0.5 g( g), 10 ml, 5 ml 0.3 mol/l,, min, 8000 r/min 20 min, 0.22 μm, 液相色谱条件及 LC-AFS 条件 -, ph 5.92, (0.45 μm), ; : 1 ml/min; : 50 r/min, : 100 ma; 330 V, 200, 8 mm, 400 ml/min, 800 ml/min 3 结果与分析 3.1 前处理条件的优化提取方法的选择 0.3 mol/l, h min 1, 18 h As III As V MMA 3, 54.70% 13.26% 85.70%, DMA 13.70%, 2 材料与方法 2.1 仪器与试剂 - ( ) ( ), (1.011±0.016) mol/g (0.233±0.005) mol/g (0.335±0.011) mol/g (0.706±0.024) mol/g;, ( ), : 2.2 试验方法溶液配制, ng/ml ( As ), LC-AFS,, 1 4 (n 3) Fig. 1 Extraction amounts of the 4 kinds of arsenics species by 2 kinds of extraction methods (n=3) 提取剂浓度的选择 ( mol/l) ( min), min, (0~0.8 mol/l), 2 DMA As III

3 9, : As V MMA, 0.3 mol/l, mol/l, 3,, 3, 0.5 mol/l, mol/l, As-III As-V, 0.3 mol/l 0.52% 0.56%, 0.3 mol/l Fig (n 3) Extraction amounts of the 4 kinds of arsenic species with different extraction time(n=3) 3.2 线性范围及检出限 2 4 (n=3) Fig. 2 Extraction amounts of the 4 kinds of arsenics species with different concentrations of nitric acid(n=3) 提取时间的选择 3.1.2, mol/l,, 3 HNO 3,, >40 min,,,, 40 min, 0.3 mol/l 4, ng/ml, 2.2, 4, 4 7 min, X, (Y), 1 0~0.1 μg/ml, 4, 0.998, (S/N=3), 0.002~0.01 μg/ml 3.3 方法准确度与精密度 20 μg/kg 4, 2.2.2, 4, 2 : 89.03%~100.70%, RSD 1.30%~4.36% Table 1 表 1 线性范围及检出限 Linear range and detection limit /min (μg/ml) (r) (μg/ml) As III ~0.100 Y=-1.674* *105 X DMA ~0.100 Y=-5.03* *104 X MMA ~0.100 Y=-5.962* *105 X As V ~0.100 Y=-3.543* *104 X

4 3676 7, 表 2 方法精密度结果 (n=6) Table 2 Precision test (n=6) (μg/kg) (μg/kg) (%) RSD(%) Fig Separation chromatogram of 4 kinds of mixed standards of arsenic species As III DMA MMA As V 样品测定 4, 3, 14, As III 0.82~36.34 μg/kg, As V 0~81.29 μg/kg, DMA MMA, 0~10.77 μg/kg 0~9.58 μg/kg (As III As V ) (200 μg/kg),, 4 结论 0.3 mol/l, min 4 :,, 1 h,, Table 3 表 3 大米样品中 4 种砷形态的测定结果 (μg/kg) Results of the 4 kinds of arsenic species in rice samples (μg/kg) As III DMA MMA As V

5 9, : 参考文献 [1] Kim JY, Kim WI, Kunhikrishnan A, et al. Determination of arsenic species in rice grains using HPLC-ICP-MS [J]. Food Sci Biotechnol, 2013, 22(6): [2] Ahmed MK, Shaheen N, Islam MS, et al. A comprehensive assessment of arsenic in commonly consumed foodstuffs to evaluate the potential health risk in Bangladesh [J]. Sci Total Environ, 2016, 544: [3] Signes-Pastor AJ, Carey M, Meharg AA. Inorganic arsenic in rice-based products for infants and young children [J]. Food Chem, 2016, 191: [4] Wahlen R HPLC-ICP- MS (AsB)[J]., 2004, 20(6): Wahlen R.. Rapid and accurate determination of AsB in fish tissue by HPLC-ICP-MS [J]. Environ Monit China, 2004, 20(6): [5],,. [J]., 2001, (2): Qian YX, Shao JZ, Wang GL. A review of principal bactierial diseases of mariculture fish [J]. Transact Oceanol Limnol, 2001, (2): [6] Mandal BK, Suzuki KT. Arsenic round the world: a review[j] Talanta, 2002, 58(1): [7] Watanabe T, Hirano S Metabolism of arsenic and its toxicological relevance [J]. Arch Toxicol, 2013, 87(6): [8] IARC. Monographs on the evaluation of carcinogenic risks to humans: Some drinking-water disinfectants and contaminants, including arsenic [C]. International Agency for Research on Cancer, 2003: [9],,,. - 5 [J]., 2010, 29(5): Lv C, Liu LP, Dong HR, et al. Analysis of five arsenic speciations by high performance liquid chromatography and inductively coupled plasma mass spectrometry [J]. J Instrum Anal, 2010, 29(5): [10],,,. - 6 [J]., 2011, 30(7): Yang LJ, Song XH, Chen LJ, et al. Simultaneous analysis of 6 arsenic speciations in fruits and vegetables by high performance liquid chromatography-inductively coupled plasma mass spectrometry [J]. Chin J Anal Lab, 2011, 30(7): [11] Llorente-Mirandes T, Barbero M, Rubio R, et al. Occurrence of inorganic arsenic in edible Shiitake (Lentinula edodes) products [J]. Food Chem, 2014, 158: [12] Melgar MJ, Alonso J, Garc a MA. Total contents of arsenic and associated health risks in edible mushrooms, mushroom supplements and growth substrates from Galicia (NW Spain) [J]. Food Chem Toxicol, 2014, 73: [13],,,. - [J]., 2014, 42(3): Chen SZ, Du Z, Liu LP, et al. Analysis of arsenic metabolites of realgar in rat viscera by HPLC-ICP-MS [J]. Chin J Anal Chem, 2014, 42(3): [14] Melgar MJ, Alonso J, García MA. Total contents of arsenic and associated health risks in edible mushrooms, mushroom pplements and growth substrates from Galicia (NW Spain) [J]. Food Chem Toxicol, 2014, 73: [15] 晞,,,. HPLC-ICP-MS [J]., 2013,(22): Chen X, He GH, Han HM, et al. Simultaneous analysis of arsenic species in selenium-enriched garlic by HPLC-ICP-MS [J]. Food Res Dev, 2013, (22): 作者简介 ( 责任编辑 : 杨翠娜 ) 魏茂琼, 研究实习员, 主要研究方向为食品安全 weimaobsyz@163.com 刘宏程, 研究员, 主要研究方向为农产品安全 liuorg@163.com

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0.

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0. 118 217 5 38 1 DOI 1.3969/j.issn.5-6521.217.1.28 Food Research And Development 1 2 1 2 1 2 1 2 1 2 1 2 1. 731 2. 731 - UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI

Microsoft Word 魏茂琼-二校 出3673

Microsoft Word 魏茂琼-二校出3673