滤过型净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼肌肉冻干粉中4种硝基呋喃类代谢物  

Determination of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder by pass-through cleanup-ultra performance liquid chromatography-triple quadrupole/compound linear ion trap mass spectrometry

作　　者：封腾望 王新新 穆树荷 周锐东 刘欢[1,2] 孙慧武 李晋成[1,2] FENG Teng-Wang;WANG Xin-Xin;MU Shu-He;ZHOU Rui-Dong;LIU Huan;SUN Hui-Wu;LI Jin-Cheng(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]中国水产科学研究院,北京100141 [2]农业农村部水产品质量安全控制重点实验室,北京100141 [3]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》2022年第13期4180-4187,共8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(2020B005);中国水产科学研究院科技创新项目(2020TD75)。

摘　　要：目的 建立一种基于滤过型净化柱净化,结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定草鱼肌肉冻干粉中4种硝基呋喃类代谢物的快速检测方法。方法 制备阴性草鱼肌肉冻干粉作为检测目标。样品经水解、衍生化并提取浓缩后,采用以50 mg C18为净化填料的CAFS clean-up净化柱对复溶液进行1次快速净化,超高效液相色谱分离,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。结果 4种硝基呋喃类代谢物在其相应的质量浓度范围内线性关系良好(r>0.999),定量限为0.6~2.4μg/kg;样品中添加定量限、2.5、5.0和50.0μg/kg浓度水平时的平均回收率在81.3%~115.1%之间,相对标准偏差为1.5%~13.1%。结论 该方法经济、简便、高效,灵敏度高,重复性好,可作为草鱼肌肉冻干粉中4种硝基呋喃类代谢物的基体标准物质的检测方法。Objective To establish a method for the rapid determination of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder based on a pass-through clean-up column combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Preparation of negative grass carp muscle lyophilized powder as the detection target.After the sample was hydrolyzed,derivatized,extracted and concentrated,the complex solution was quickly purified by CAFS clean-up column with 50 mg C18 as purification filler,separated by ultra performance liquid chromatography,determined by triple quadrupole/compound linear ion trap mass spectrometer,and quantitatively analyzed by internal standard method.Results The linear relationships of the 4 kinds of nitrofuran metabolites were good within the corresponding mass concentrations(r>0.999),and limits of quantification were 0.6-2.4 μg/kg.The average recoveries of samples at spiked levels(the limit of quantification,2.5,5.0,50.0 μg/kg) were 81.3%-115.1%,the relative standard deviations were 1.5%-13.1%.Conclusion This method has the advantages of economy,simplicity,high efficiency,high sensitivity and good repeatability.It can be used for the determination of matrix reference material of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder.

关 键 词：草鱼肌肉冻干粉 硝基呋喃类代谢物 滤过型净化柱 超高效液相色谱-串联质谱法 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]