ICP-MS技术同时测定多种食品添加剂中二十一种元素
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摘要
建立一种高通量、高灵敏度可同时测定多种食品添加剂中21种元素的ICP-MS方法。测定过程中,使用内标法校正和碰撞反应池消除质谱干扰技术。针对汞易扩散和Hg~(2+)的歧化反应而不稳定的特点,采用添加金溶液的方法,对测定条件进行优化,最终确定溶液中金浓度为60μg/L时达到最优的测定条件。与以往的测定方法相比具有前处理简单、测定速度快、灵敏度高、可同时测定21种元素等明显优势。检出限为0.001～0.011mg/kg,线性相关系数为0.9993以上,精密度RSD≤7.35,加标回收率在94.8%～106%之间。
A method for simultaneous determination of 21 elements in food additives by ICP-MS with high throughput and high sensitivity was established. In the process of determination,the internal standard correction and collision reaction pool technique were used to further eliminate the mass spectrometry interference. For the easy diffusion of mercury and the instability of the disproportionation reaction of Hg~(2+),the method of adding gold solution was used to optimize the determination conditions and finally determine the optimal determination conditions when the gold concentration is 60μg/L in the solution. Compared with the previous methods,this method has the obvious advantages of simple pretreatment,fast determination,high sensitivity and simultaneous determination of 21 elements. The detection limit is 0.001 mg/kg ～ 0.011 mg/kg,the linear correlation coefficient is more than 0.9993,the precision RSD is less than 7.35,and the recovery rate is between 94.8% ～ 106%.
A method for simultaneous determination of 21 elements in food additives by ICP-MS with high throughput and high sensitivity was established. In the process of determination,the internal standard correction and collision reaction pool technique were used to further eliminate the mass spectrometry interference. For the easy diffusion of mercury and the instability of the disproportionation reaction of Hg~(2+),the method of adding gold solution was used to optimize the determination conditions and finally determine the optimal determination conditions when the gold concentration is 60μg/L in the solution. Compared with the previous methods,this method has the obvious advantages of simple pretreatment,fast determination,high sensitivity and simultaneous determination of 21 elements. The detection limit is 0.001 mg/kg ～ 0.011 mg/kg,the linear correlation coefficient is more than 0.9993,the precision RSD is less than 7.35,and the recovery rate is between 94.8% ～ 106%.
引文
[1]中华人民共和国卫生部.GB 2760-2014食品安全国家标准食品添加剂使用标准[S].北京:国家卫生与计划生育委员会,2015.
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[4]Javed Nawab,Saad Farooqi,Wang Xiaoping,Sardar Khan,Asad Khan.Levels,dietary intake,and health risk of potentially toxic metals in vegetables,fruits,and cereal crops in Pakistan[J].Environmental Science and Pollution Research,2018(25):24111-24124.
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[10]邱倩.石墨炉原子吸收法测定食品中镍的方法的建立[J].医学动物防制,2015,31(9):1057-1059.
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[14]Aanassova D,Stefanova V,Russeva E.Co-precipitative pre-concentration with sodium and ICP-AES diethyldithiocarbamate determination of Se,Cu,Pb,Zn,Fe,Co,Ni,Mn,Cr and Cd in water[J].Talanta,1998(47):1 237.
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[16]赵小学,赵宗生,王玲玲.水中汞的电感耦合等离子体-质谱法测定[J].中国测试,2013,39(6):50-52.
[17]张秀武,李永华,杨林生,等.温控湿法消化ICP-MS法测定全血中的铅硒砷汞[J].光谱学与光谱分析,2010,30(7):1972-1974.
[18]宋旭,孔牟恒,高峰.HPLC-ICP-MS法分析测定药用植物中的形态汞[J].现代仪器与医疗,2013,19(2):1-4.
[19]张兰,陈玉红,施燕支,等.高效液相色谱-电感耦合等离子体质谱联用技术测定二价汞、甲基汞、乙基汞与苯基汞[J].环境化学,2009,28(5):772-774.
[20]袁媛,周雨,王涛.电感耦合等离子体质谱法加L-半胱氨酸及金测定汞[J].中国卫生检验杂志,2016,26(14):2025-2029.
[21]史潜玉,刘立,柯润辉,等.ICP-MS在食品质量安全领域应用研究进展[J].食品与发酵工业,2012,38(12):118-124.
[22]符靓.八极杆碰撞/反应池-ICP-MS法测定果脯中的重金属元素[J].食品工业科技,2012,33(15):311-314.
[23]杜鉴,薛毅.食品添加剂中重金属元素前处理与检测方法研究进展[J].食品工业科技,2015,36(04):397-399.
[24]张宏康,王中瑗,蔡斯斯.ICP-MS测定食品及相关产品中重金属等元素的研究进展[J].食品研究与开发,2016,37(17):195-200.
[25]聂西度,梁逸曾,符靓,等.电感耦合等离子体质谱法测定甜味剂中重金属元素[J].光谱学与光谱分析,2012,32(10):2838-2841.
[26]雷超海,秦愫妮.ICP-OES/ICP-MS测定食品添加剂碳酸钙中15种杂质元素[J].中国食品添加剂,2017(6):204-208.
[27]江波,黄建华,刘伟.电感耦合等离子体串联质谱法测定野生皂荚中多种微量元素[J].光谱学与光谱分析,2017,37(12):3859-3864.
[2]王静,孙宝国.食品添加剂与食品安全[J].科学通报,2013,58(26):2619-2625.
[3]LUO Li-qiang,SHEN Ya-ting,WANG Xiao-fang,CHUBin-bin,XU Tao,LIU Ying,ZENG Yuan,LIU Jian.Phytoavailability,bioaccumulation,and human health risks of metal(loid)elements in an agroecosystem near a lead-zinc mine[J].Environmental Science and Pollution Research,2018(25):24111-24124.
[4]Javed Nawab,Saad Farooqi,Wang Xiaoping,Sardar Khan,Asad Khan.Levels,dietary intake,and health risk of potentially toxic metals in vegetables,fruits,and cereal crops in Pakistan[J].Environmental Science and Pollution Research,2018(25):24111-24124.
[5]胡斌,江祖成,等.色谱-原子光谱/质谱联用技术及形态分析[M].北京科学出版社,2005:6-9.
[6]杨慧芬,李明元,等.食品理化检验标准手册[M].北京中国标准出版社,1987:97.
[7]孙丽丽.电感耦合等离子体光谱测定磷酸中铅、砷、镉、铬[J].磷肥和复肥,2012,27(3):72.
[8]苗春雨.食品中铬的测定方法改进[J].中国医药指南,2013,17(11):86-87.
[9]叶瑞洪,陈孝堪.食品中镉的测定方法研究[J].福建师范大学学报,2009,91(2):20-25.
[10]邱倩.石墨炉原子吸收法测定食品中镍的方法的建立[J].医学动物防制,2015,31(9):1057-1059.
[11]李启隆,冯晓红,等.铅-二甲酚橙配合物吸附波及食糖中铅的测定[J].环境化学,1989,8(4):57.
[12]杨振华.Pb(Ⅱ)-KI-罗丹明B离子缔合物萃取光度法测定皮蛋中的微量铅[J].理化检验-化学分册,1999,35(1):35.
[13]Shigehiro K,Yasuko A,Kiyoshi H.Separation and concen-tration of trace lead by coprecipitation with yttrium phosphate[J].Chemistry Letters,2000(19):208.
[14]Aanassova D,Stefanova V,Russeva E.Co-precipitative pre-concentration with sodium and ICP-AES diethyldithiocarbamate determination of Se,Cu,Pb,Zn,Fe,Co,Ni,Mn,Cr and Cd in water[J].Talanta,1998(47):1 237.
[15]Ltif E,Ugur S.Sibel O.Determination of trace amounts of some metals in samples with high salt content by atomic absorption spectrometry after cobalt-diethyldithiocarbama tecoprecipitation[J].Talanta,1997(44):1017.
[16]赵小学,赵宗生,王玲玲.水中汞的电感耦合等离子体-质谱法测定[J].中国测试,2013,39(6):50-52.
[17]张秀武,李永华,杨林生,等.温控湿法消化ICP-MS法测定全血中的铅硒砷汞[J].光谱学与光谱分析,2010,30(7):1972-1974.
[18]宋旭,孔牟恒,高峰.HPLC-ICP-MS法分析测定药用植物中的形态汞[J].现代仪器与医疗,2013,19(2):1-4.
[19]张兰,陈玉红,施燕支,等.高效液相色谱-电感耦合等离子体质谱联用技术测定二价汞、甲基汞、乙基汞与苯基汞[J].环境化学,2009,28(5):772-774.
[20]袁媛,周雨,王涛.电感耦合等离子体质谱法加L-半胱氨酸及金测定汞[J].中国卫生检验杂志,2016,26(14):2025-2029.
[21]史潜玉,刘立,柯润辉,等.ICP-MS在食品质量安全领域应用研究进展[J].食品与发酵工业,2012,38(12):118-124.
[22]符靓.八极杆碰撞/反应池-ICP-MS法测定果脯中的重金属元素[J].食品工业科技,2012,33(15):311-314.
[23]杜鉴,薛毅.食品添加剂中重金属元素前处理与检测方法研究进展[J].食品工业科技,2015,36(04):397-399.
[24]张宏康,王中瑗,蔡斯斯.ICP-MS测定食品及相关产品中重金属等元素的研究进展[J].食品研究与开发,2016,37(17):195-200.
[25]聂西度,梁逸曾,符靓,等.电感耦合等离子体质谱法测定甜味剂中重金属元素[J].光谱学与光谱分析,2012,32(10):2838-2841.
[26]雷超海,秦愫妮.ICP-OES/ICP-MS测定食品添加剂碳酸钙中15种杂质元素[J].中国食品添加剂,2017(6):204-208.
[27]江波,黄建华,刘伟.电感耦合等离子体串联质谱法测定野生皂荚中多种微量元素[J].光谱学与光谱分析,2017,37(12):3859-3864.
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