摘要
采用改良QuEChERS技术作为前处理方法,建立了水产品中扑草净及其代谢物残留的超高效液相色谱-串联质谱分析方法。样品用乙腈提取,经增强型脂质去除吸附剂与Cleanert LipoNo组合净化,采用选择反应监测正离子模式测定,内标法定量。结果表明:扑草净及其代谢物在1.0~500 ng/mL质量浓度范围内线性关系良好,确定系数R2大于0.992,方法检出限和定量限分别低至0.20μg/kg和0.50μg/kg,在草鱼、克氏原螯虾和中华绒螯蟹等基质的加标实验中呈现良好的准确度与精密度,平均加标回收率和相对标准偏差分别为74.4%~113.7%和3.17%~11.47%。经内标法校正,5种扑草净及其代谢物在不同水产品中的基质效应不明显。方法实现了水产品中扑草净及其代谢物的识别与定量分析,并通过检测药浴扑草净的克氏原螯虾阳性样品验证了方法的适用性。
An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of the residues of prometryn and its metabolites in aquatic products was developed using a modified quick,easy,cheap,effective,rugged and safe(QuEChERS)method for sample pretreatment.Homogenized samples were extracted with acetonitrile and purified by the combined use of enhanced matrix removal of lipids(EMR-Lipid)and Cleanert LipoNo.The detection was carried out in the positive ion mode with selected reaction monitoring(SRM)and the internal standard method was selected for quantification.Under the optimal conditions,the calibration curves for prometryn and its four metabolites were linear with correlation coefficient(R2)above 0.992 in the concentration range of 1–500 ng/mL.The limits of detection(LODs)and limits of quantitation(LOQs)for all analytes were as low as 0.20 and 0.50μg/kg,respectively.For spiked grass carp,crayfish and Chinese mitten crab,good accuracy and precision were observed,with average recoveries and relative standard deviations(RSDs)ranging from 74.4%to 113.7%and 3.17%to 11.47%,respectively.After correction by the internal standard method,the matrix effects of the five compounds in different aquatic products were not significant.The developed method allows the identification and quantitative analysis of the residues of prometryn and its metabolites in aquatic products.Additionally,the applicability of this method was validated by detecting positive samples of crayfish bathed with prometryn.
作者
彭婕
穆迎春
喻亚丽
陈建武
刘婷
何力
甘金华
PENG Jie;MU Yingchun;YU Yali;CHEN Jianwu;LIU Ting;HE Li;GAN Jinhua(Fishery Quality Supervision and Testing Center of Ministry of Agriculture and Rural Affairs,Fishery Products Quality Safety Risk Assessment Laboratory(Wuhan)of Ministry of Agriculture and Rural Affairs,Yangtze River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Wuhan 430223,China;Chinese Academy of Fishery Sciences,Beijing 100141,China;Key Laboratory of Control of Quality and Safety for Aquatic Products of Ministry of Agriculture and Rural Affairs,Beijing 100141,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2024年第3期185-192,共8页
Food Science
基金
现代农业产业技术体系建设专项(CARS-48)
中国水产科学研究院基本科研业务项目(2020TD74)
“十三五”国家重点研发计划重点专项(2019YFD0901700)。
关键词
超高效液相色谱-串联质谱
水产品
扑草净
代谢物
QUECHERS
ultra-high performance liquid chromatography-tandem mass spectrometry
aquatic products
prometryn
metabolites
quick,easy,cheap,effective,rugged and safe
