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

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

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.