壳聚糖净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定水产品中硝基呋喃类代谢物残留研究  

Determination of nitrofuran metabolites in aquatic products by chitosan purification-ultra performance liquid chromatography-quadrupole linear ion trap-mass spectrometry

作　　者：霍文迪 文宇鹏 张荣月[1] 李晋成[2,3] HUO Wen-Di;WEN Yu-Peng;ZHANG Rong-Yue;LI Jin-Cheng(School of New Materials and Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617,China;Chinese Academy of Fishery Sciences,Beijing 100141,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture,Beijing 100141,China;College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China)

机构地区：[1]北京石油化工学院新材料与化工学院,北京102617 [2]中国水产科学研究院,北京100141 [3]农业农村部水产品质量安全控制重点实验室,北京100141 [4]上海海洋大学水产与生命学院,上海201306

出　　处：《食品安全质量检测学报》2025年第7期71-77,共7页Journal of Food Safety and Quality

基　　金：中央级公益性科研院所基本科研业务费项目(2025XT04);国家现代农业产业技术体系项目(CARS-48);中国水产科学研究院科技创新项目(2020TD75)。

摘　　要：目的建立一种基于壳聚糖净化结合超高效液相色谱-三重四极杆/复合线性离子阱质谱法,测定水产品中硝基呋喃类代谢物残留的快速检测方法。方法样品经盐酸水解、2-硝基苯甲醛衍生、乙酸乙酯提取、壳聚糖净化、氮吹浓缩复溶后,借助超高效液相色谱仪实现快速分离,三重四极杆/复合线性离子阱质谱仪进行测定,内标法定量分析,实现快速、准确地测定水产品中硝基呋喃类代谢物残留量。结果4种硝基呋喃类代谢物在0.5~10.0μg/L质量浓度范围内线性关系良好,相关系数均大于0.998,定量限为0.5μg/kg;以鲤鱼、大菱鲆以及南美白对虾为样品,在3个不同添加水平下4种硝基呋喃类代谢物的平均回收率为96.5%~116.5%,日内相对标准偏差为2.2%~9.3%,日间相对标准偏差为2.7%~9.7%。结论该方法经济、简便、高效,灵敏度高,重复性好,可作为水产品中4种硝基呋喃类代谢物残留的常规检测方法。Objective To develop a rapid method for the determination of nitrofuran metabolites in aquatic products based on chitosan purification combined with ultra performance liquid chromatography and triple quadrupole/composite linear ion trap mass spectrometer.Methods The samples were hydrolyzed by hydrochloric acid,derived by 2-nitrobenzaldehyde,extracted by ethyl acetate,rapidly purified by chitosan,and then concentrated and redissolved.Rapid separation was achieved by ultra performance liquid chromatography,measured by triple quadrupole/composite linear ion trap mass spectrometer,and quantified by internal standard method to achieve the rapid and accurate determination of nitrofuran metabolites residues in aquatic products.Results The 4 kinds of nitrofuran metabolites had a good linear relationship in the concentration range of 0.5–10.0μg/L,the correlation coefficients were all more than 0.998,and the limit of quantification was 0.5μg/kg.Taking carp,Scophthalmus maximus and Litopenaeus vannamei as samples,the average recovery of 4 kinds of nitrofuran metabolites at 3 different addition levels was 96.5%–116.5%,the intra-day relative standard deviation was 2.2%–9.3%,and the intra-day relative standard deviation was 2.7%–9.7%.Conclusion The method is economical,simple,efficient,sensitive and reproducible,and can be used as a routine method for the determination of 4 kinds of nitrofuran metabolites in aquatic products.

关 键 词：壳聚糖 水产品 硝基呋喃类代谢物 超高效液相色谱-三重四极杆/复合线性离子阱质谱法 

分 类 号：R28[医药卫生—中药学]