鱼中氯芬新残留检测方法建立及食用安全性分析  

Establishment of a method for detection of lufenuron residues in fish and analysis of food safety

作　　者：王继耀 程江峰 WANG Ji-yao;CHENG Jiang-feng(School of Marine Science and Bioengineering,Qingdao University of Science and Technology,Qingdao 266042,Shandong,China;Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality,Ministry of Agriculture and Rural Affairs,Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071,Shandong,China;Pilot(Qingdao)National Laboratory for Marine Science and Technology,Qingdao 266237,Shandong,China)

机构地区：[1]青岛科技大学,海洋科学与生物工程学院,山东青岛266042 [2]农业农村部水产品质量安全检测与评价重点实验室,中国水产科学研究院黄海水产研究所,山东青岛266071 [3]青岛海洋科学与技术试点国家实验室,山东青岛266237

出　　处：《淡水渔业》2023年第6期31-36,共6页Freshwater Fisheries

基　　金：国家重点研发计划“蓝色粮仓科技创新”重点专项“水产品危害物质检测与质量控制技术(2019YFD0901701)”。

摘　　要：为了解我国水产品中氯芬新残留状况,本研究采用QuEChERS样品进行前处理技术,建立了鱼中氯芬新残留高效液相色谱-串联质谱检测方法,并利用该技术首次对采自5个省市13个品种128个鱼类样品中氯芬新残进行检测;分别参照欧盟规定的氯芬新在鲑中最大残留限量1350μg/kg,以及在部分动物源性食品中最大残留限量20μg/kg,采用风险熵值法(RQ)进行氯芬新残留食用安全性风险分析。研究结果显示:氯芬新在0.5~100.0 ng/mL浓度范围内线性关系良好,线性相关系数(r^(2))大于0.995,检出限为1.0μg/kg。在1.0、2.0、5.0、50.0μg/kg四个添加水平上进行加标回收实验,平均回收率在79.16%~106.33%之间,相对标准偏差在1.63%~7.26%之间(n=6)。在鳙、鲤、鲫、鲟、虹鳟、鲢、鳊、鳜和大菱鲆中均未检出氯芬新残留,表明这些品种的鱼类氯芬新残留食用风险很小。在加州鲈、草鱼、大黄鱼和乌鳢中氯芬新最大残留含量分别为343.02、58.43、33.19μg/kg和1.38μg/kg,检出率分别为37.21%、29.41%、40.00%和16.67%。据欧盟动物源性食品中氯芬新最大残留限量,乌鳢氯芬新残留食用为低风险,草鱼、大黄鱼和加州鲈均为高风险,其中加州鲈RQ值是风险值的17倍之多。综上结果表明在我国部分鱼类养殖过程中可能存在较为严重的氯芬新违规使用现象,存在较高氯芬新食用安全风险。Due to the illegal use and abuse of lufenuron in fish culture,it is easy to cause harm to aquatic organisms and affect consumers through the food chain.In this study,we established a method for detecting lufenuron residues.We used the technique to test and perform a risk assessment of lufenuron residues in 13 species of fish samples in China for the first time.It is expected to provide technical support and reference for the status and potential safety risk analysis of lufenuron residues in aquatic products in China.A high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was developed for the determination of lufenuron residues in fish using the QuEChERS method as a pretreatment.A total of 128 samples of 13 species of fish from 5 provinces were tested for lufenuron residues.Concerning the EU maximum residue limits(MRLs)of 1350μg/kg for lufenuron in sea bass and 20μg/kg in some foods of animal origin,the risk-entropy method was used to analyze the safety of lufenuron residues in food.The results showed that the linearity of lufenuron was good in the concentration range of 0.5~100.0 ng/mL,with the linear correlation coefficient(r^(2))greater than 0.995 and the detection limit was 1.0μg/kg.The average recoveries ranged from 79.16%to 106.33%at four fill levels of 1.0,2.0,5.0 and 50.0μg/kg,with the relative standard deviations ranging from 1.63%to 7.26%(n=6).Lufenuron residues were not detected in Aristichthys nobilis,Cyprinus carpio,Carassius auratus,Acipenser sinensis,Oncorhynchus mykiss,Hypophthalmichthys molitrix,Parabramis pekinensis,Siniperca chuatsi and Scophthalmus maximus,indicating that therewas little risk of consumption of lufenuron residues in these species of fish.The maximum residue levels of lufenuron in Micropterus salmoides,Ctenopharyngodon idellus,Larimichthys crocea,and Channa argus were 343.02μg/kg,58.43μg/kg,33.19μg/kg and 1.38μg/kg,and the detection rates were 37.21%,29.41%,40.00%and 16.67%,respectively.According to the EU maximum residue limit in food of anim

关 键 词：氯芬新 残留 高效液相色谱-串联质谱法 食品安全分析 

分 类 号：S912[农业科学—水产科学]