免疫亲和柱净化-液相色谱-串联质谱法同时测定水产品中8种霉菌毒素  

Simultaneous Determination of 8 Mycotoxins in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Immunoaffinity Column Clean-up

作　　者：李益丰 张秋云 杨洪生[2,3] 朱晓华 沈美芳[2] 陈慧敏 LI Yifeng;ZHANG Qiuyun;YANG Hongsheng;ZHU Xiaohua;SHEN Meifang;CHEN Huimin(College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China;Freshwater Fishery Research Institute of Jiangsu Province,Nanjing 210017,China;Jiangsu Aquatic Product Quality Inspection Center,Nanjing 210017,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd.,Shanghai 200335,China)

机构地区：[1]上海海洋大学水产与生命学院,上海201306 [2]江苏省淡水水产研究所,江苏南京210017 [3]江苏省水产质量检测中心,江苏南京210017 [4]上海爱博才思分析仪器贸易有限公司,上海200335

出　　处：《食品工业科技》2023年第7期294-300,共7页Science and Technology of Food Industry

基　　金：江苏现代农业产业技术体系建设项目(JATS[2021]368);江苏省“333高层次人才培养工程”项目(BRA2020374)。

摘　　要：目的:建立免疫亲和柱净化-液相色谱-串联质谱法(LC-MS/MS)同时测定水产品中8种霉菌毒素残留。方法:样品经乙腈水溶液(84:16,V:V)提取,多毒素免疫亲和柱净化。色谱柱为Agilent Proshell 120 SB·C_(18)(2.1 mm×100 mm,2.7μm),流动相为甲醇-5 mmol/L乙酸铵(含0.1%甲酸),梯度洗脱,流速为0.4 mL/min,柱温为40℃。采用电喷雾离子源正负离子同时扫描,多反应监测模式(MRM)进行质谱检测。结果:8种霉菌毒素在1.0~50.0 ng/mL范围内线性关系良好(R2>0.992),方法检出限在0.05~0.50μg/kg之间,定量限在0.17~1.65μg/kg之间;8种霉菌毒素加标回收率在75.6%~106.3%之间,相对标准偏差(RSD)为3.5%~9.3%。结论:该方法操作便捷、灵敏度高、准确可靠,能满足水产品中多种霉菌毒素残留快速检测需求。Objective:A liquid chromatography-tandem mass spectrometry coupled with immunoaffinity column clean-up method was established for the determination of 8 mycotoxins in aquatic products.Methods:The samples were extracted with acetonitrile water(84:16,V:V),and purified by multifunctional immunoaffinity columns.The chromatographic column was Agilent Proshell 120 SB·C_(18)column(2.1 mm×100 mm,2.7 μm).Mobile phase was methanol and 5 mmol/L ammonium acetate(containing 0.1% formic acid),gradient elution.The flow rate was 0.4 mL/min,and the column temperature was 40 ℃.The electrospray was operated in both positive and negative mode at the same time,and the samples were detected by multiple reaction monitoring mode(MRM).Results:The linear relations of the eight mycotoxins were good within the concentration range of 1.0~50.0 ng/mL(R~2>0.992).The limits of detection were between 0.05~0.50 μg/kg,and the limits of quantification were between 0.17~1.65 μg/kg.The average recoveries were 75.6%~106.3%,and the relative standard deviations(RSDs) were 3.5%~9.3%.Conclusion:The method is simple,sensitive and accurate for the rapid analysis of mycotoxin residues in aquatic products.

关 键 词：霉菌毒素 水产品 液相色谱-串联质谱法 免疫亲和柱 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]