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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
夏明星,黄均艳,李光满,陈忠祥,孙涛,李应国
0
(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)
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10 μg·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
DOI:10.13610/j.cnki.1672-352x.20170524.011
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。
The establishment of a detection method for detecting melamine in animal-derived blood
XIA Mingxing,HUANG Junyan,LI Guangman,CHEN Zhongxiang,SUN Tao,LI Yingguo
(Wanzhou Entry-Exit Inspection and Quarantine Bureau,Wanzhou 404000;Chongqing Vocational Institute of Safety Technology,Wanzhou 404000;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.
Key words:  melamine  mass spectrometry  animal-derived blood

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