动物性食品中氯化亚汞、硝酸亚汞和醋酸汞的总汞残留测定方法研究
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摘要
建立了经微波消解法处理样品,氢化物发生-原子荧光光谱法(HG-AFS)测定动物性食品中氯化亚汞、硝酸亚汞和醋酸汞的总汞残留分析方法.样品经过微波消解系统处理,用硼氢化钾作为还原剂,盐酸作为载流,采用氢化物发生-原子荧光光谱仪进行总汞含量的测定.结果表明:动物性食品中汞质量浓度与响应值在0.05～2.00μg/L范围内呈现良好的线性关系(r>0.9990).氯化亚汞、硝酸亚汞和醋酸汞的检出限分别为0.004、0.001和0.006μg/L;定量限分别为0.010、0.003和0.020μg/L;最低检出质量分数分别为1.00、0.25和1.50μg/kg;相对精密度(RSD)分别为3.82%、3.27%和4.11%;平均回收率范围分别为89.07%～110.08%、80.17%～113.10%和89.83%～112.77%.
A microwave digestion,hydride generation-atomic fluorescence spectrometer method for determining the total mercury residues of mercurous chloride,mercurous nitrate and mercuric acetate in animal derived food was established.The samples were pretreated with microwave digestion and determination by hydride generation-atomic fluorescence spectrometer,with the potassium borohydride as the reductant,and the hydrochloric acid as current-carrying.The density of mercury and its response value was in good linearity over the range of 0.05-2.00 μg / L(r > 0.999 0).As for mercurous chloride,mercurous nitrate and mercuric acetate,the limit of detection was 0.004,0.001 and 0.006 μg / L respectively,the limit of quantification was 0.010,0.003 and 0.020 μg / L respectively,the minimum detectable concentration was 1.00,0.25 and 1.50 μg / kg respectively,the relative standard deviation(RSD) was 3.82%,3.27% and 4.11% respectively.The average recovery was 89.07%-110.08%,80.17% 113.10% and 89.83%-112.77% respectively.
A microwave digestion,hydride generation-atomic fluorescence spectrometer method for determining the total mercury residues of mercurous chloride,mercurous nitrate and mercuric acetate in animal derived food was established.The samples were pretreated with microwave digestion and determination by hydride generation-atomic fluorescence spectrometer,with the potassium borohydride as the reductant,and the hydrochloric acid as current-carrying.The density of mercury and its response value was in good linearity over the range of 0.05-2.00 μg / L(r > 0.999 0).As for mercurous chloride,mercurous nitrate and mercuric acetate,the limit of detection was 0.004,0.001 and 0.006 μg / L respectively,the limit of quantification was 0.010,0.003 and 0.020 μg / L respectively,the minimum detectable concentration was 1.00,0.25 and 1.50 μg / kg respectively,the relative standard deviation(RSD) was 3.82%,3.27% and 4.11% respectively.The average recovery was 89.07%-110.08%,80.17% 113.10% and 89.83%-112.77% respectively.
引文
[1]中华人民共和国卫生部,中国国家标准化管理委员会.GB/T500917—2003食品中总汞及有机汞的测定[S].北京:中华人民共和国卫生部,中国国家标准化管理委员会,2003.
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[9]乔凌霞.原子荧光法同时测定砷、汞混合水样[J].医学动物防制,2010,26(3):288-290.
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[14]耿勇超,王建滨,付艳慧.微波消解-原子荧光光度法测定土壤中汞[J].江苏环境科技,2008,21(增刊1):58-59.
[15]刘双德.双道原子荧光光度计同时测定化妆品中砷和汞[J].现代预防医学,2010,37(7):1336-1337.
[16]李红芸,田海燕,李明艳.氢化物原子荧光分光光度法测定化妆品中微量汞[J].中国卫生检验杂志,2009,19(4):804-805.
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[18]蔡秋.氢化物原子荧光光谱法测定水产品中的痕量汞[J].光谱实验室,2003,20(1):98-101.
[19]鲍华.氢化物原子荧光光度法同时测定食品中砷和汞[J].河南预防医学杂志,2008,19(1):22-23.
[20]王颖.氢化物原子荧光光度法测定食品中汞的探讨[J].中国卫生检验杂志,2010,20(10):2632-2633.
[21]陈彩燕,梁群珍,林坤立.微波消解-氢化物发生-原子荧光法测定肉及肉制品中汞[J].中国卫生检验杂志,2010,20(5):1021-1022.
[22]徐燕.微波消解-氢化物发生原子荧光光度法测定食品中的砷和汞[J].预防医学论坛,2008,14(1):47-48.
[23]王铁良,司敬沛,张玲,等.微波消解-原子荧光光谱法快速测定食品中汞和砷的方法研究[J].河南农业科学,2010(2):128-131.
[24]方兰云,王立.微波消解-原子荧光光谱法测定大米中的痕量汞[J].中国卫生检验杂志,2010,20(3):519-521.
[25]刘雨.氢化物发生-原子荧光法同时测定砷和硒、铬和汞的研究及应用[D].济南:山东大学,2010.
[26]刘铭,刘凤枝,蔡彦明.土壤中总汞砷铅的氢化物发生-原子荧光法的研究[J].农业环境与发展,2004,21(6):42-44.
[2]郑礼胜,王士龙,安红.双硫腙水相分光光度法测定废水中汞[J].环境监测管理与技术,1996,8(3):32-33.
[3]孙引,郑建明.原子荧光法检测鸡肉中铅、砷、汞[J].广州化工,2011,39(6):117-119.
[4]王安俊,郎春燕.微波消解冷原子荧光法测定市售猪肉中的痕量汞[J].广东微量元素科学,2005,12(12):44-46.
[5]魏中文.利用冷原子吸收法在原子吸收分光光度计上测定水样汞[J].云南环境科学,2004,23(51):204-205.
[6]唐莲仙,丁亚明.冷原子荧光光谱法测定化妆品中汞[J].中国测试技术,2007,33(1):133-135.
[7]杨秀琳.原子荧光光谱法测定水中的痕量砷、硒、汞[J].化学分析计量,2004,13(1):32-34.
[8]童俊,臧道德.双道原子荧光光谱法测定水中痕量Hg、As、Se、Sb[J].净水技术,2004,23(6):27-29.
[9]乔凌霞.原子荧光法同时测定砷、汞混合水样[J].医学动物防制,2010,26(3):288-290.
[10]陆文娟.顺序注射氢化物发生原子荧光光度法测定水中As、Se、Sb、Hg[J].现代仪器,2007,13(6):81-82.
[11]栗云霞,李伟国,陆安祥,等.原子荧光光谱法同时测定土壤中的砷和汞[J].安徽农业科学,2009,37(12):5344-5346.
[12]董大鹏.氢化物发生原子荧光光谱法测定土壤中的汞[J].广州化工,2009,37(8):176-178.
[13]李艳.氢化物发生-原子荧光光谱法测定土壤中的汞[J].光谱实验室,2004,21(4):831-832.
[14]耿勇超,王建滨,付艳慧.微波消解-原子荧光光度法测定土壤中汞[J].江苏环境科技,2008,21(增刊1):58-59.
[15]刘双德.双道原子荧光光度计同时测定化妆品中砷和汞[J].现代预防医学,2010,37(7):1336-1337.
[16]李红芸,田海燕,李明艳.氢化物原子荧光分光光度法测定化妆品中微量汞[J].中国卫生检验杂志,2009,19(4):804-805.
[17]刘裕婷,朱力.原子荧光光谱法同时测定食品中汞和锡[J].中国卫生检验杂志,2008,18(7):1308-1309.
[18]蔡秋.氢化物原子荧光光谱法测定水产品中的痕量汞[J].光谱实验室,2003,20(1):98-101.
[19]鲍华.氢化物原子荧光光度法同时测定食品中砷和汞[J].河南预防医学杂志,2008,19(1):22-23.
[20]王颖.氢化物原子荧光光度法测定食品中汞的探讨[J].中国卫生检验杂志,2010,20(10):2632-2633.
[21]陈彩燕,梁群珍,林坤立.微波消解-氢化物发生-原子荧光法测定肉及肉制品中汞[J].中国卫生检验杂志,2010,20(5):1021-1022.
[22]徐燕.微波消解-氢化物发生原子荧光光度法测定食品中的砷和汞[J].预防医学论坛,2008,14(1):47-48.
[23]王铁良,司敬沛,张玲,等.微波消解-原子荧光光谱法快速测定食品中汞和砷的方法研究[J].河南农业科学,2010(2):128-131.
[24]方兰云,王立.微波消解-原子荧光光谱法测定大米中的痕量汞[J].中国卫生检验杂志,2010,20(3):519-521.
[25]刘雨.氢化物发生-原子荧光法同时测定砷和硒、铬和汞的研究及应用[D].济南:山东大学,2010.
[26]刘铭,刘凤枝,蔡彦明.土壤中总汞砷铅的氢化物发生-原子荧光法的研究[J].农业环境与发展,2004,21(6):42-44.