渔业研究2024，Vol.46Issue(5)：528-538,11.DOI:10.14012/j.jfr.2024085
改良QuEChERS技术测定水产品中甲胺磷残留及不确定度评定
Determination and uncertainty evaluation of methamidophos residues in aquatic products by modified QuEChERS technique
摘要
Abstract
[Objective]This study aimed to accurately assess the quality and safety level of aquatic products in the national rice-fishery symbiosis system,ensuring the safety of aquatic products for consumption and main-taining the healthy and sustainable development of the fishery industry.[Methods]Rice paddy aquatic products such as Procambarus clarkii,Cyprinus carpio and Eriocheir sinensis were chosen as the sample mat-rix,and the organophosphorus insecticide methamidophos was selected as the research object.The good chro-matographic separation and sufficient mass spectrometry response intensity of methamidophos were used to screen the suitable conditions for instrumental determination.Based on the modified QuEChERS technique,the optimal preparation method was preferred by comparatively analyzing the effects of different extraction solvents,such as acetonitrile,ethyl acetate,acidified acetonitrile,acidified ethyl acetate,and different combina-tions of purification reagents,including PSA,C18,anhydrous magnesium sulphate,and Cleanert LipoNo,as well as different nitrogen blowing temperatures on the recoveries of spiked methamidophos.Finally,an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the accurate determination of methamidophos residues in aquatic products.Its measurement uncertainty introduced by sample preparation and instrumental analysis were evaluated at the same time,which provided the basis for optimizing the determination procedure and improving the accuracy of the test data.[Results]The preparation optimization experiments suggested that the analytes were preferably extracted with acetonitrile,purified by Cleanert LipoNo,concentrated by nitrogen blowing at 40℃,separated on a Waters Acquity UPLC BEH C18 column and quantified by external standard method.Under the optimal conditions,the standard curve was lin-ear in the range of 0.1-50.0 µg·L-1 with the correlation coefficient of 0.999 2.The limits of detection and quan-tification were found to be 0.25 µg·kg-1 and 0.5 µg·kg-1.Due to the thorough sample preparation,the recoveries were 82.1%-96.5%with relative standard deviations less than 11%.In this study,the main sources of uncer-tainty in measurement were standard curve fitting and recoveries,followed by standard solution preparation,sample repeated measurement,sample weighing and sample processing.The error caused by volumetric determ-ination was the least.[Conclusion]Due to the advantages of low matrix interference and better sensitivity than existing literature reports,this method aims to precisely determine the trace residues of methamidophos in aquatic products.During the detection process,it is necessary to control the influence of standard curve fitting and recoveries on the accuracy of the results,so as to scientifically evaluate the residual concentration of meth-amidophos in aquatic products and dietary risk.关键词
甲胺磷/水产品/QuEChERS/超高效液相色谱-串联质谱/测量不确定度Key words
methamidophos/aquatic products/QuEChERS/ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/measurement uncertainty分类
农业科技引用本文复制引用
彭婕,喻亚丽,程波,张浪,甘金华,何力..改良QuEChERS技术测定水产品中甲胺磷残留及不确定度评定[J].渔业研究,2024,46(5):528-538,11.基金项目
中国水产科学研究院中央级公益性科研院所基本科研业务费(2023TD79) （2023TD79）
中央级科研院所基本科研业务费(2023XT0704) （2023XT0704）
"十三五"国家重点研发计划重点专项(2019YFD0901700) （2019YFD0901700）
国家重点研发计划(2022YFF0608202) （2022YFF0608202）
国家现代农业产业技术体系项目(CARS-46) （CARS-46）
