微波消解-电感耦合等离子体质谱法测定酱油中的铅和钠含量
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摘要
目的建立微波消解和电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)联用同时测定酱油中高含量元素钠(Na)和低含量元素铅(Pb)的检测方法。方法根据酱油高盐分性质,选取合适同位素和电子稀释参数、采用碰撞池He模式及内标校正等技术消除干扰,用微波消解对样品进行前处理,采用电感耦合等离子体质谱仪同时检测Na和Pb含量。结果 Na和Pb在0~800 mg/L、0~25μg/L质量浓度范围内线性关系良好,其线性相关系数均为0.9992,Pb和Na的检出限分别为0.02、3 mg/kg,相对标准偏差(relative standard deviation,RSD)小于5%,回收率为96.2%~112%。结论此方法能有效消除干扰,准确、简便、快速,适用于酱油中Pb和Na的同时测定。
Objective To establish a method for determination of sodium and lead in soy sauce by inductively coupled plasma mass spectrometry(ICP-MS). Methods According to the high salinity of soy sauce, appropriate isotope and electronic dilution parameters were selected, He mode of collision cell and internal standard correction were used to eliminate interference. The sample was pretreated by microwave digestion, and contents of Na and Pb were simultaneously detected by inductively coupled plasma mass spectrometry. Results Na and Pb had good linear relationships in the rage of 0-800 mg/L and 0-25 μg/L, respectively, and the linear correlation coefficients were both 0.9992. The limits of detection of Pb and Na were 0.02 and 3 mg/kg, respectively. The relative standard deviations(RSDs) were less than 5%, and the recoveries were 96.2%-112%. Conclusion This method can effectively eliminate interference, and is accurate, simple and rapid, which is suitable for simultaneous determination of Pb and Na in soy sauce.
Objective To establish a method for determination of sodium and lead in soy sauce by inductively coupled plasma mass spectrometry(ICP-MS). Methods According to the high salinity of soy sauce, appropriate isotope and electronic dilution parameters were selected, He mode of collision cell and internal standard correction were used to eliminate interference. The sample was pretreated by microwave digestion, and contents of Na and Pb were simultaneously detected by inductively coupled plasma mass spectrometry. Results Na and Pb had good linear relationships in the rage of 0-800 mg/L and 0-25 μg/L, respectively, and the linear correlation coefficients were both 0.9992. The limits of detection of Pb and Na were 0.02 and 3 mg/kg, respectively. The relative standard deviations(RSDs) were less than 5%, and the recoveries were 96.2%-112%. Conclusion This method can effectively eliminate interference, and is accurate, simple and rapid, which is suitable for simultaneous determination of Pb and Na in soy sauce.
引文
[1]刘静.酱油中铅含量测定方法的研究[J].宿州学院学报,2006,(5):83-84.Liu J.Study on the determination of lead content in soy sauce[J].J Suzhou Univ,2006,(5):83-84.
[2]GB 2762-2017食品安全国家标准食品中污染物限量[S].GB 2762-2017 National food safety standard-Limits of contaminants in food[S]
[3]王放.食品营养保健原理与技术[M].北京:中国轻工业出版社,1996.Wang F.The principle and technology of food nutrition and health care[M].Beijing:China Light Industry Press,1996.
[4]赵发,刘艳明,张喜琦,等.石墨炉原子吸收法测定酱油中铅方法改进[J].中国调味品,2017,(9):142-144.Zhao F,Liu YM,Zhang XQ,et al.Improvement of method for testing lead in soy sauce by graphite furnace atomic absorption spectrometry[J].China Cond,2017,(9):142-144.
[5]朱静,王静静,代国栋,等.原子吸收光谱法测定超细粉末中钠的含量[J].农业灾害研究,2017,(6):58-62.Zhu J,Wang JJ,Dai GD,et al.Determination of sodium in ultrafine powder by atomic absorption spectrometry[J].J Agric Catastr,2017,(6):58-62.
[6]李敏,连晓文,姚敬,等.电感耦合等离子体-质谱法测定酱油中12种金属[J].中国食品卫生杂志,2014,(4):344-347.Li M,Lian XW,Yao J,et al.Determination method of 12 metals in soy sauce by ICP-MS[J].Chin J Food Hyg,2014,(4):344-347.
[7]林立,陈玉红,田艳玲,等.电感耦合等离子体质谱法直接测定酱油中的铅[J].环境化学,2007,(3):410-412.Lin L,Chen YH,Tian YL,et al.Direct determination of lead in soybean sauce by using ICP-MS[J].Environ Chem,2007,(3):410-412.
[8]彭荣飞,侯建荣,黄聪.ICP-MS直接测定酱油中Pb和As的研究[J].中国卫生检验杂志,2008,(7):1315-1316.Peng RF,Hou JR,Huang C.Direct determination of lead and arsenic in sauce by inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(7):1315-1316.
[9]汪晓冬.微波消解-电感耦合等离子质谱法对8种市售酱油无机元素的分析[J].食品研究与开发,2010,(11):159-161.Yang J.Determination of inorganic elements of 8 soy sauces in Chinese market by ICP-MS with microwave digestion[J].Food Res Dev,2010,(11):159-161.
[10]彭寨玉,杜二青,徐淑暖,等.电感耦合等离子体质谱法直接测定酱油中铅[J].中国卫生检验杂志,2008,(11):2275-2276.Peng ZY,Du EQ,Xu SN,et al.Direct determination of lead in soybean sauce by using inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(11):2275-2276.
[11]刘奋,戴京晶,林奕芝,等.ICP-MS测定食品中多种金属元素[J].现代预防医学,2002,(1):43-45.Liu F,Dai JJ,Lin YZ,et al.Determination of multi-elements in food of ICP-MS[J].Mod Prev Med,2002,(1):43-45.
[12]Melaku S,Dams R,Moens L.Determination of trace elements in agricultural soil samples by inductively coupled plasma-mass spectrometry:Microwave acid digestion versus aqua regia extraction[J].Ana Chim Acta,2005,543(1):117-123.
[13]母清林,方杰,佘运勇,等.在线稀释/预浓缩-电感耦合等离子体质谱法分析海水中11种痕量元素[J].分析化学,2015,(9):1360-1365.Mu QL,Fang J,She YY,et al.Determination of trace metals in seawater by inductively coupled plasma mass spectrometry with on-line injection technique[J].Chin J Anal Chem,2015,(9):1360-1365.
[14]彭荣飞,黄聪,卓召模,等.碰撞池ICP-MS测定近海海水中的Cr、As、Se、Cd、Cu、Zn、Hg和Pb[J].中国卫生检验杂志,2008(12):2529-2531,2542.Peng RF,Huang C,Zhuo ZM,et al.Determination of Cr,As,Se,Cd,Cu,Zn,Hg and Pb in offing seawater by collision cell inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(12):2529-2531,2542.
[15]李清清,赵艳菊,施敬文.微波消解-电感耦合等离子体质谱法测定坚果中钒、钴、钼含量[J].食品安全质量检测学报,2017,(4):1450-1454.Li QQ,Zhao YJ,Shi JW.Determination of vanadium,cobalt and molybdenum in nuts by inductively coupled plasma mass spectrometry with microwave digestion[J].J Food Saf Qual,2017,(4):1450-1454.
[2]GB 2762-2017食品安全国家标准食品中污染物限量[S].GB 2762-2017 National food safety standard-Limits of contaminants in food[S]
[3]王放.食品营养保健原理与技术[M].北京:中国轻工业出版社,1996.Wang F.The principle and technology of food nutrition and health care[M].Beijing:China Light Industry Press,1996.
[4]赵发,刘艳明,张喜琦,等.石墨炉原子吸收法测定酱油中铅方法改进[J].中国调味品,2017,(9):142-144.Zhao F,Liu YM,Zhang XQ,et al.Improvement of method for testing lead in soy sauce by graphite furnace atomic absorption spectrometry[J].China Cond,2017,(9):142-144.
[5]朱静,王静静,代国栋,等.原子吸收光谱法测定超细粉末中钠的含量[J].农业灾害研究,2017,(6):58-62.Zhu J,Wang JJ,Dai GD,et al.Determination of sodium in ultrafine powder by atomic absorption spectrometry[J].J Agric Catastr,2017,(6):58-62.
[6]李敏,连晓文,姚敬,等.电感耦合等离子体-质谱法测定酱油中12种金属[J].中国食品卫生杂志,2014,(4):344-347.Li M,Lian XW,Yao J,et al.Determination method of 12 metals in soy sauce by ICP-MS[J].Chin J Food Hyg,2014,(4):344-347.
[7]林立,陈玉红,田艳玲,等.电感耦合等离子体质谱法直接测定酱油中的铅[J].环境化学,2007,(3):410-412.Lin L,Chen YH,Tian YL,et al.Direct determination of lead in soybean sauce by using ICP-MS[J].Environ Chem,2007,(3):410-412.
[8]彭荣飞,侯建荣,黄聪.ICP-MS直接测定酱油中Pb和As的研究[J].中国卫生检验杂志,2008,(7):1315-1316.Peng RF,Hou JR,Huang C.Direct determination of lead and arsenic in sauce by inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(7):1315-1316.
[9]汪晓冬.微波消解-电感耦合等离子质谱法对8种市售酱油无机元素的分析[J].食品研究与开发,2010,(11):159-161.Yang J.Determination of inorganic elements of 8 soy sauces in Chinese market by ICP-MS with microwave digestion[J].Food Res Dev,2010,(11):159-161.
[10]彭寨玉,杜二青,徐淑暖,等.电感耦合等离子体质谱法直接测定酱油中铅[J].中国卫生检验杂志,2008,(11):2275-2276.Peng ZY,Du EQ,Xu SN,et al.Direct determination of lead in soybean sauce by using inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(11):2275-2276.
[11]刘奋,戴京晶,林奕芝,等.ICP-MS测定食品中多种金属元素[J].现代预防医学,2002,(1):43-45.Liu F,Dai JJ,Lin YZ,et al.Determination of multi-elements in food of ICP-MS[J].Mod Prev Med,2002,(1):43-45.
[12]Melaku S,Dams R,Moens L.Determination of trace elements in agricultural soil samples by inductively coupled plasma-mass spectrometry:Microwave acid digestion versus aqua regia extraction[J].Ana Chim Acta,2005,543(1):117-123.
[13]母清林,方杰,佘运勇,等.在线稀释/预浓缩-电感耦合等离子体质谱法分析海水中11种痕量元素[J].分析化学,2015,(9):1360-1365.Mu QL,Fang J,She YY,et al.Determination of trace metals in seawater by inductively coupled plasma mass spectrometry with on-line injection technique[J].Chin J Anal Chem,2015,(9):1360-1365.
[14]彭荣飞,黄聪,卓召模,等.碰撞池ICP-MS测定近海海水中的Cr、As、Se、Cd、Cu、Zn、Hg和Pb[J].中国卫生检验杂志,2008(12):2529-2531,2542.Peng RF,Huang C,Zhuo ZM,et al.Determination of Cr,As,Se,Cd,Cu,Zn,Hg and Pb in offing seawater by collision cell inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2008,(12):2529-2531,2542.
[15]李清清,赵艳菊,施敬文.微波消解-电感耦合等离子体质谱法测定坚果中钒、钴、钼含量[J].食品安全质量检测学报,2017,(4):1450-1454.Li QQ,Zhao YJ,Shi JW.Determination of vanadium,cobalt and molybdenum in nuts by inductively coupled plasma mass spectrometry with microwave digestion[J].J Food Saf Qual,2017,(4):1450-1454.