Determination of Residual Amount of Melamine in Foodstuffs by Hyphenation of Liquid Chromatography and Mass Spectrometry in Tandem
摘 要
提出了液相色谱-串联质谱联用法测定动物源性食品中三聚氰胺残留量的方法.样品采用乙腈进行提取,饱和氯化钠溶液进行分配经反相色谱分离后,串联质谱法进行测定,同位素内标法进行定量,方法的测定下限(10S/N)为0.05 mg·kg-1,以5类食品样品为基体,加入4种不同浓度水平的三聚氰胺标准作回收试验,测得回收率在72.9%~104.1%之间,测定值的相对标准偏差(n=6)在4.7%~15.2%之间.
Abstract
It was reported that residual amount of melamine in foodstuffs of animal origin was determined by LC-MS/MS. Melamine was separated from the sample,in which standard melamine labelled with 15N3 was added as internal standard,by extraction with acetonitrile and partitioned with saturated sodium chloride solution. After centrifugation,an aliquot of the supernatant was taken for separation by reverse phase liquid chromatography and the content of melamine was determined by MS/MS. Lower limit of determination (10S/N) of the method was found to be 0.05 mg·kg-1. Tests for recovery were made by addition of standard melamine at 4 different concentration levels to 5 kinds of foodstuffs as matrixes,values of recovery found were in the range of 72.9%-104.1%,with values of RSD′s (n=6) in the range from 4.7% to 15.2%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目
收稿日期 2009/3/20
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备注夏崇菲(1981-),女,上海人,硕士研究生,从事理化分析检验研究.
引用该论文: XIA Chong-fei,ZHAO Shan-zhen,HAN Li,GUO De-hua,DENG Xiao-jun,CHEN Shun-sheng. Determination of Residual Amount of Melamine in Foodstuffs by Hyphenation of Liquid Chromatography and Mass Spectrometry in Tandem[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(12): 1361~1364
夏崇菲,赵善贞,韩丽,郭德华,邓晓军,陈舜胜. 液相色谱-串联质谱联用法测定食品中三聚氰胺残留量[J]. 理化检验-化学分册, 2009, 45(12): 1361~1364
被引情况:
【1】马云云,谭金峰,徐玉文,王洪涛,李佳,李源, "液相色谱-高分辨质谱法测定壮阳类保健品中非法添加物",理化检验-化学分册 51, 325-330(2015)
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参考文献
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【10】GB/T 22388-2008原料乳与乳制品中三聚氰胺检测方法[S].
【2】林祥梅,王建峰,贾广乐,等.三聚氰胺的毒性研究[J].毒理学杂志,2008,22(3):216.
【3】ANDERSEN W C,TURNIPSEED S B. Determination of melamine residues in catfish tissue by triple quadrupole LC-MS-MS with HILIC chromatography[J]. Laboratory Information Bulletin,2007,23:4396.
【4】李爱军,张代辉,马书民,等.液相色谱-串联质谱法测定饲料中三聚氰胺残留[J].分析化学,2008,36(5):699.
【5】栾伟.液相色谱串联质谱法(LC-MS/MS)分析宠物食品中三聚氰胺[J].分析测试学报,2007,26:285.
【6】蔡勤仁,欧阳颖瑜,钱振杰,等.超高效液相色谱-电喷雾串联质谱法测定饲料中残留的三聚氰胺[J].色谱,2008,26(3):339.
【7】SANCHO J V,IBEZ M. Residue determination of cyromazine and its metabolite melamine in chard samples by ion-pair liquid chromatography coupled to electrospray tandem mass spectrometry[J]. Analytica Chimica Acta,2005,530:237.
【8】丁涛,徐锦忠,李健忠,等.高效液相色谱-二极管阵列检测法及高效液相色谱-电喷雾串联质谱法测定植物源性蛋白中残留的三聚氰胺[J].色谱,2008,26(1):6.
【9】何强,孔祥虹,李建华,等.离子交换色谱-紫外检测法测定乳制品中三聚氰胺[J].中国乳品工业,2008,36(6):55.
【10】GB/T 22388-2008原料乳与乳制品中三聚氰胺检测方法[S].
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