超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物

超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物
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。

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.

标题：超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物
英文标题：Determination of metabolites of nitrofuran in shrimp using ultra pressure liquid chromatography-tandem mass spectrometry

作者：
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

中文关键词:硝基呋喃,代谢物,超高压液相色谱-串联质谱,虾,
英文关键词:nitrofuran,metabolite,ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),shrimp,

发表日期：2012-11-13

超高压液相色谱-串联质谱法测定虾中硝基呋喃代谢物.pdf

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