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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
【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1 350μg/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。
【Abstract】 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 1350 μg/kg for lufenuron in sea bass and 20 μg/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(r2)greater than 0.995 and the detection limit was 1.0 μg/kg.The average recoveries ranged from 79.16% to 106.33% at four fill levels of 1.0,2.0,5.0 and 50.0 μg/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 343.02 μg/kg, 58.43 μg/kg, 33.19 μg/kg and 1.38 μg/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 animal origin, Channa argus is low risk, Ctenopharyngodon idellus,Larimichthys crocea,and Micropterus salmoides are high risk, especially California perch RQ value is as much as 17 times of the risk value, indicating that there is a risk of consumption of lufenuron residues in sea bass, there may be more severe violations of the use of lufenuron in some fish farming process in China.
【Key words】 lufenuron; residue; high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS); food safety risk analysis;
- 【文献出处】 淡水渔业 ,Freshwater Fisheries , 编辑部邮箱 ,2023年06期
- 【分类号】TS254.7
- 【下载频次】27