杨奕,邵兵.超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物[J].食品安全质量检测学报,2013,4(1):135-140
超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物
Determination of metabolites of nitrofuran in shrimp using ultra pressure liquid chromatography-tandem mass spectrometry
投稿时间:2012-11-13  修订日期:2013-01-08
DOI:
中文关键词:  硝基呋喃  代谢物  超高压液相色谱-串联质谱  
英文关键词:nitrofuran  metabolite  ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  shrimp
基金项目:国家高技术研究发展计划(863计划)项目(2010AA023001)、北京市卫生系统高层次卫生技术人才培养计划项目
作者单位
杨奕 北京市疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室 
邵兵 北京市疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室 
AuthorInstitution
YANG Yi Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Bejing Center for Disease Prevention and Control 
SHAO Bing Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control 
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中文摘要:
      目的 建立虾中四种硝基呋喃代谢物的超高压液相色谱-串联四极杆质谱(UPLC-MS/MS)分析方法。方法 样品经2-NB衍生, HLB固相萃取柱净化、富集; 以乙腈?5 mmol/L乙酸铵(含0.1%乙酸)为流动相, 在正离子模式下, 采用多反应监测(MRM)方式进行检测。结果 四种硝基呋喃代谢物的定量限(LOQ)均为1.0 μg/kg, 三个添加水平(1.0、5.0、20.0 μg/kg)的平均回收率在81.6%~95.1%之间, 相对标准偏差均小于13.6%。结论 本方法适用于虾中污染物残留检测。
英文摘要:
      Objective An analytical method for the detection of four metabolites of nitrofuran in shrimp by ultra- perssure liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) was established. Methods After derived by 2-NB, the sample extraction was purified by HLB cartridge. The objective compounds were separated using Waters Acquity BEH C18 column with acetonitrile –5 mmol/L ammonium acetate (0.1% acetic acid) as mobile phase and analyzed by UPLC-MS/MS under multiple reaction monitoring mode(MRM). Results The LOQ for four target compounds were 1.0 μg/kg. The average recoveries were 81.6%~95.1% at the level of 1.0, 5.0 μg/kg and 20.0 μg/kg with the relative standard deviation lower than 13.6%. Conclusion The method is suitable for the detection of residual pollutant in shrimp.
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