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动物源血液中三聚氰胺的液相色谱质谱联用检测方法的建立
引用本文:夏明星,黄均艳,李光满,陈忠祥,孙涛,李应国.动物源血液中三聚氰胺的液相色谱质谱联用检测方法的建立[J].安徽农业大学学报,2017,44(3):392-397.
作者姓名:夏明星  黄均艳  李光满  陈忠祥  孙涛  李应国
作者单位:万州出入境检验检疫局,万州,404000;重庆安全技术职业学院,万州,404000;重庆出入境检验检疫局,重庆,400000
基金项目:重庆市应用开发计划项目(cstc2014yykfB80016)和国家认证认可监督管理委员会2014年第三批出入境检验检疫行业标准制修订计划项目(2014B368)共同资助。
摘    要:为建立不同动物源血液中三聚氰胺的质谱联用检测方法,通过研究不同提取溶剂提取效率和不同固相萃取柱净化能力,进行回收率、精密度和检出限等技术要素评价。分析得到,以甲醇:水:乙酸溶液(49.5:49.5:1)作为提取试剂,MCX柱作为净化固相萃取柱,各种动物源血液样品中三聚氰胺回收率为90.0%~110%,精密度RSD为0.96%~4.64%,方法定量限为10μg·kg~(-1)。试验表明此方法灵敏度高,稳定性好,适用于动物血液样品中三聚氰胺有机物含量的检测。

关 键 词:三聚氰胺  质谱联用  动物源血液

The establishment of a detection method for detecting melamine in animal-derived blood
XIA Mingxing,HUANG Junyan,LI Guangman,CHEN Zhongxiang,SUN Tao and LI Yingguo.The establishment of a detection method for detecting melamine in animal-derived blood[J].Journal of Anhui Agricultural University,2017,44(3):392-397.
Authors:XIA Mingxing  HUANG Junyan  LI Guangman  CHEN Zhongxiang  SUN Tao and LI Yingguo
Institution:Wanzhou Entry-Exit Inspection and Quarantine Bureau,Wanzhou 404000,Chongqing Vocational Institute of Safety Technology,Wanzhou 404000,Wanzhou Entry-Exit Inspection and Quarantine Bureau,Wanzhou 404000,Wanzhou Entry-Exit Inspection and Quarantine Bureau,Wanzhou 404000,Chongqing Entry-Exit Inspection and Quarantine Bureau,Chongqing 400000 and Chongqing Entry-Exit Inspection and Quarantine Bureau,Chongqing 400000
Abstract:In order to establish a Mass spectrometry method for determination of melamine in animal-derived blood,we investigated the extraction efficiency of various solvents and the purification ability of different SPE columns and evaluated the technical parameters including recovery rate,precision and detection limit.With the 49.5:49.5:1 (methanol:water:acetic acid) solution as an extraction reagent and using MCX column as purifying solid-phase extraction column,the melamine in animal blood samples of recovery ranged from 90.0% to 110.0%;the precision RSD was in the range of 0.96 %-4.64%;and the detection limit was 10 μg.kg-1.The result indicated that this optimized method was sensitive and stable,which could be potentially applied to determination of melamine in animal blood samples.
Keywords:melamine  mass spectrometry  animal-derived blood
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