陕西省水产品中4种硝基呋喃代谢物的检测

Determination of four nitrofurans metabolites residues in aquatic products in Shaanxi Province

【目的】对陕西省市售水产品中4种硝基呋喃代谢物进行检测,为保证当地食品安全提供依据。【方法】从陕西西安、宝鸡、安康、延安、咸阳、渭南、商洛、铜川、汉中和榆林共10个地市的超市和农贸市场随机采集16种120份鱼样品,将样品匀浆后在酸性条件下用2-硝基苯甲醛避光振荡衍生16h,Oasis HLB固相萃取柱提取、净化,超高效液相色谱-串联质谱法检测,同位素内标法定量,统计水产品中呋喃唑酮代谢物3-氨基-2-噁唑烷基酮(AOZ)、呋喃它酮代谢物5-甲基-吗啉-3-氨基-2-噁唑烷基酮(AMOZ)、呋喃妥因代谢物1-氨基-2-内酰脲(AHD)和呋喃西林代谢物氨基脲(SEM)的检测结果,分析样品中硝基呋喃类药物的残留情况。【结果】4种硝基呋喃代谢物的总检出率为6.5%,呋喃唑酮代谢物检出率最高,为8.3%;16种水产品中4种硝基呋喃代谢物残留的样品检出率为15.0%;16种鱼品种的检出率为37.5%,其中武昌鱼、罗非鱼、草鱼、鲶鱼、鲤鱼和鲫鱼检出率依次为100.0%,100.0%,20.6%,15.4%,15.2%和6.3%,其余鱼样未检出;草鱼中4种代谢物的平均含量远高于其他鱼种;咸阳、商洛、延安、渭南、宝鸡和西安的检出率分别为22.9%,20.8%,8.3%,8.3%,2.1%和2.1%;咸阳的草鱼、商洛的鲤鱼、渭南的草鱼和鲤鱼在养殖或运输过程中有使用多种硝基呋喃类药物的情况。【结论】陕西省部分地区、部分鱼种中硝基呋喃类药物残留水平超标,草鱼、鲤鱼、鲶鱼和鲫鱼等当地养殖的鱼类安全性较低,应引起有关食药监部门的重视。

【Objective】The purpose of the study was to determine levels of four nitrofurans metabolites residues in commercial aquatic products in Shaanxi Province,and provide reference for food security.【Method】A total of 16 kinds of 120 fish samples were collected randomly from major supermarkets and farmers markets in Xi＇an,Baoji,Ankang,Yan＇an,Xianyang,Weinan,Shangluo,Tongchuan,Hanzhong and Yulin,in Shaanxi Province.After being homogenated,16 hderivation was conducted with 2-nitrobenzaldenhyde under acidic condition.Extraction and purification were conducted by Oasis HLB solid phase extraction column,and concentrations of four nitrofurans metabolites residues in samples were quantified by ultra-performance liquid,chromatography-tandem mass spectrometry（UPLC-MS/MS）,and isotope internal standard method.The detection results of furazolidone metabolites 3-amino-2-oxalidone（AOZ）,furaltadonemetabolites 5-morpholinomethyl-3-amino-2-oxalidinone（AMOZ）,nitrofurantoin metabolites 1-amino-hydantoin（AHD）,and nitrofurazone metabolites semicarbazide（SEM）in aquatic products were counted,and illegal use of nitrofurans drugs in aquaculture was analyzed.【Result】The total detection rate of four nitrofurans metabolites was 6.5%,and that of furazolidone metabolites 3-amino-2-oxalidone（AOZ）was the highest of 8.3%.The detection rate of samples in 16 kinds of aquatic products was 15.0%.The detection rate of fish species was 37.5% with the rates in bluntnose block bream,tilapia,grass carp,catfish,carp,and crucian carp of 100.0%,100.0%,20.6%,15.4%,15.2% and 6.3%,respectively,while they were not detectable in other fish samples.The mean levels of four nitrofurans metabolites in grass carp were higher than other fish species.The detection rates of four nitrofurans metabolites in Xianyang,Shangluo,Yan＇an,Weinan,Baoji,and Xi＇an were 22.9%,20.8%,8.3%,8.3%,2.1% and 2.1%,respectively.Mixed use of nitrofurans drugs was found in grass carp from Xianyang,carp from Shangluo,and in grass carp and carp from Weinan.【Conclusion】Levels of nitrofurans drugs residues in some aquatic products of some areas were higher than the standards in Shaanxi Province.The security levels of grass carp,carp,catfish and crucian carp were low and attention should be paid by food and drug supervision and administration department.