【摘要】 建立了中华绒螯蟹中硝基呋喃类代谢物残留量的液相色谱—串联质谱检测方法.取均质后的中华绒螯蟹可食部分样品,用盐酸水解组织中蛋白结合代谢物,经2-硝基苯甲醛37℃过夜衍生化,调节pH值至约7.0～7.4后,用乙酸乙酯提取,正己烷净化.选用电喷雾离子源,在正离子、多反应监测方式模式下进行定性,以同位素内标法进行定量.方法的检出限为0.5μg.kg-1,工作曲线的线性范围为1.25～50.0μg.L-1.在添加浓度为0.5～10.0μg.kg-1的范围内,AMOZ、SEM、AHD和AOZ的回收率分别在92.8%～106%、84.5%～94.6%、80.6%～98.6%和88.4%～105%之间,相对标准偏差均小于10%.更多还原

【Abstract】 A high-performance liquid chromatography-tandem mass spectrometric method is established for the determination of metabolites of nitrofurans residues in Chinese Mitten Crab.Homogenized edible samples are hydrolyzed and derivatized using 2-nitrobenzaldehyde at 37℃ overnight followed by addition of internal standards.After adjusting the pH to 7.0~7.4,the solution is extracted twice by ethyl acetate.The residue is dissolved with 1.0mL dissolvant solution(acetontrile:0.4% acetic acid solution=10:90) and defatted with n-hexane(saturated by acetonitrile).The four analytes are separated on ZORBAX Eclipse XDB-C18 Column,and finally identified by Electrospray ionization-tandem mass spectrometry(ESI-MS-MS)analysis.Analytic confirmation is performed using multi-reaction monitoring(MRM) with one precursor ion and two product ions as identifiers.Analytes quantification is performed using internal standard method.The quantitative limit of the method is 0.5 μg.kg-1.and the linear range is 0.25~10.0μg.kg-1.The recovery range of AMOZ is 92.8%~106%,SEM is 84.5%~94.6%,AHD is 80.6%~98.6%,AOZ is 88.4%~105%,when fortified at the concentration of 0.5 μg.kg-1,1 μg.kg-1,2 μg.kg-1 and 10.0 μg.kg-1.The RSD of the method is less than 10%.更多还原