ICP-MS Determination of Inorganic Arsenic in Meat Food with IC Separation
摘 要
粉碎的肉类食品试样用水分散后经超声提取40 min,于提取液中加乙酸(3+97)使蛋白质沉淀析出,并在4 ℃用高速离心法予以分离.取上层清液用经0.45 μm滤膜过滤,滤液中的无机砷(Ⅲ及Ⅴ)和有机胂,即甲基胂(MA)和二甲基胂(DMA)通过IonPac AS 18阴离子色谱柱予以分离.用不同浓度的氢氧化钾溶液作流动相进行梯度淋洗,使上述4种形态的砷在碱性溶液中分别以阴离子状态而分离.用电感耦合等离子体质谱法分别测定洗脱液中无机砷(Ⅲ及Ⅴ)的含量,两者的检出限依次为0.3,0.5 μg·kg-1.以肉类食品为基体加入3种不同浓度的标准溶液,按试验方法分析后求得方法的回收率及精密度为① 三价砷回收率在83.1%~93.3%之间,相对标准偏差(n=6)在3.3%~6.7%之间;② 五价砷回收率在85.3%~97.6%之间,相对标准偏差(n=6)为3.1%~5.9%.
Abstract
Sample of ground meat was dispersed with water,and extracted ultrasonically for 40 min.Acetic acid (3+97) was added to the extract to precipitate protein which was separated by high speed centrifugation at 4 ℃.The supernatant was taken and filtered on 0.45 μm filtering membrane.IonPac AS 18 anion chromagraphic column was used for separation of inorganic arsenic (Ⅲ and Ⅴ) and organic arsenic compounds of methylarsine (MA) and dimethylarsine (DMA).Potassium hydroxide solutions of different concentrations were used as mobile phase in gradient elution of the 4 species of arsenic in forms of their anions,in the alkaline solutions.The eluates were used for ICP-MS determination of inorganic As(Ⅲ) and As(Ⅴ),with values of detection limits (3S/N) of 0.3 and 0.5 μg·kg-1,respectively.Tests for recovery and precision were made by standard addition method at 3 different concentration levels,the results obtained were as follows: ① for As(Ⅲ),recovery 83.1% to 93.3%,RSD′s (n=6) 3.3% to 6.7%;② for As(Ⅴ),recovery 85.3% to 97.6%,RSD′s (n=6) 3.1% to 5.9%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 福建省科技计划重点项目(2008Y03010822)资助
收稿日期 2009/7/16
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备注黄红霞(1965-),女,福建福州人,高级工程师,主要从事食品、饲料、化工产品的检测及管理工作.
引用该论文: HUANG Hong-xia. ICP-MS Determination of Inorganic Arsenic in Meat Food with IC Separation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(10): 1122~1124
黄红霞. 离子色谱分离-电感耦合等离子体质谱联用法测定肉类食品中无机砷[J]. 理化检验-化学分册, 2010, 46(10): 1122~1124
被引情况:
【1】斯 文,钱翠珠,林 垦,朱书秀,陆明华, "电感耦合等离子体质谱法测定烟用接装纸中砷时内标法和标准加入法的比较",理化检验-化学分册 51, 1552-1556(2015)
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参考文献
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【3】李卫华,王雅珍,刘玉海.高效液相色谱-电感耦合等离子体质谱检测海藻中的砷[J].陕西师范大学学报:自然科学版,2006,34(7):65-68.
【4】滕曼,梁立娜,蔡亚岐,等.离子色谱-氢化物发生原子荧光光谱联用技术在砷形态分析中的应用[J].分析试验室,2007,26(1):22-25.
【5】罗锡明,赵立谦,徐步县.离子色谱氢化物发生原子荧光法测定含金尾矿中砷[J].光谱学与光谱分析,2008,28(1):206-208.
【6】韦昌金,刘霁欣,裴晓华.离子交换色谱氢化物发生双道原子荧光法同时测定砷和硒形态[J].分析化学,2008,36(8):1061-1065.
【7】张国平,刘虹,刘丛强,等.离子色谱-等离子体质谱联用测定热泉水样的砷形态[J].分析试验室,2007,26(9):17-20.
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