2013年陕西市售水产品中孔雀石绿和结晶紫的检测

Determination of malachite green and crystal violet residues in aquatic products of Shaanxi in 2013

【目的】对2013年陕西省市售水产品中的4种兽药残留进行检测研究,为保证当地食品安全提供参考。【方法】随机抽取16种购自陕西省10个地市批发市场的120份鱼样品,采集鱼样可食部分匀浆后用乙腈提取,经中性氧化铝净化,采用超高效液相色谱-串联质谱法对兽药孔雀石绿、结晶紫及其代谢产物隐性孔雀石绿、隐性结晶紫的残留情况进行检测和定性、定量分析,统计4种兽药残留的总检出率、16种样品中兽药残留的检出率、10个地市兽药残留的检出率、4种兽药残留的平均水平及同一样品中4种兽药的混配使用情况。【结果】16种120份鱼肉样品中4种兽药的总检出率为4.6%,其中隐性结晶紫未检出;120份鱼肉样品兽药残留的样品检出率为15.8%,其中梭边鱼、鲑鱼、鲤鱼、鲶鱼和草鱼兽药残留的检出率分别为100.0%,100.0%,33.3%,15.4%和11.8%,高于2011年的全国平均水平(9.0%),其余11种鱼样中未检出兽药残留;除榆林外的9个地市市售鱼样中均检出兽药残留,其中商洛、咸阳的检出率最高,均为10.4%;来自商洛的鲶鱼样品同时检出多种兽药残留,说明商洛存在多种兽药混配使用现象。【结论】陕西省市售水产品中4种兽药残留的总检出率并不高,但市场占有率较高的鲤鱼、鲶鱼、草鱼样品中均有兽药残留,且检出率均较高;10个地市中有9个地市市售水产品中均有兽药检出,且存在多种兽药混配使用情况,对人体健康具有潜在威胁,应当引起重视。

【Objective】This study determined residual levels of 4veterinary drugs in aquatic products in Shaanxi in 2013 to ensure food security.【Method】A total of 120 fish samples for 16 types were collected from wholesale markets in 10 cities of Shaanxi Province.After homogenate was collected,the veterinary drugs were extracted by acetonitrile and cleaned up by neutral alumina.The concentrations of total malachite green and crystal violet and their metabolites residues were detected by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and qualitatively and quantitatively analyzed.The total detection rates of 4veterinary drugs,detection rates of 16 samples,detection rates of samples in 10 cities,mean levels of veterinary drugs residues and the detection rates of mixed veterinary drugs were coun-ted.【Result】The total detection rate of 4veterinary drugs was 4.6% and leuco crystal violet was not detected.The detection rate in 16 kinds of samples was 15.8%,and those of spindle edge fish,trout,carp,catfish,and grass carp samples were 100.0%,100.0%,33.3%,15.4%,and 11.8%,respectively,higher than the mean level in China(9.0%).None of veterinary drugs was detected in other 11 kinds of samples.Veterinary drugs were detected in 9areas except Yulin,with the highest detection rates of 10.4%in Shangluo and Xianyang.Various veterinary drugs were detected simultaneously in the samples from Shangluo,indicating abuse of mixed veterinary drugs.【Conclusion】The detection rates of 4veterinary drugs residue in aquatic products were not high in Shaanxi Province.However,the high presence of drugs in carp,catfish,and grass carp samples in 9areas and mixed abuse of veterinary drugs poses potential threat to human health,which high attention should be paid to.