摘要
采用超高效液相色谱-串联质谱法测定鱼肉中AHD、AMOZ、AOZ、SEM残留。样品经盐酸水解,与2-NB在37℃水浴中衍生16 h后,离心,加入0.5 mol/L磷酸氢二钾2 mL,用氢氧化钠调节pH至7.1~7.5之间,乙酸乙酯萃取,氮吹,流动相定容。采用电喷雾MRM正离子模式扫描,内标法定量。4种代谢物在2.5μg/kg^50μg/kg的浓度范围内有良好的线性关系,相关系数大于0.999 3,最低检出限为0.2μg/kg。在样品中加入(1、10、20μg/kg)3个浓度水平,平均回收率83.0%~101%之间,相对标准偏差(RSD_(n=6))在4.2%~11.3%之间。使用同位素内标法定量,校正了衍生不完全、光照分解、溶液p H对提取效率的影响,提高了定量结果的准确性,适用于鱼肉中4种硝基呋喃代谢物的确证。
AHD, AMOZ, AOZ, SEM residues in fish were detected by ultra performance liquid chromatogra- phy - tandem mass spectrometry. The samples were hydrolyzed by hydrochloric acid, was derivated by 2-NB at 37 ℃ after 16 h and then added with 2 mL 0.5 mol/L dipotassium hydrogen phosphate, adjusted pH to 7.1-7.5 with sodium hydroxide, extracted by ethyl acetate, nitrogen evaporated, the mobile phase volumed. Electro- spray ionization source was applied and operated in positive ion mode, using MRM scanning and internal stan- dard method for quantitative analysis. Four metabolites showed a good linear correlation between 2.5 μg/kg to 50 μg/kg concentration with range coefficient greater than 0.999 3 and the lowest detection limit 0.2 μg/kg. The average recovery （n=6） of the samples at three levels （ 1,10,20 μg/kg） relative standard deviation between 4.2 % and 11.3 %.The method used ranged from 83.0 % to 101% with the isotope internal standard for determi- nation which corrected influence of incomplete derivation, decomposition by the light and solution pH on the extraction efficiency and improved the accuracy of quantitative results. The method was applicable to screening and confirmation of four nitrofuran metabolites in fish.
出处
《食品研究与开发》
CAS
北大核心
2016年第10期159-164,共6页
Food Research and Development
关键词
硝基呋喃代谢物
鱼
超高效液相色谱—串联质谱法
nitrofuran metabolites
fish
ultra performance liquid chromatography-tandem mass spectrometry
