QuEChERS-液相色谱-串联质谱法测定水产品中双甲脒及其代谢物残留量  

Determination of amitraz and its metabolite residues in aquatic products by QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：郭灿 王守英 黄志英[1] 白冰[1] 邹艺 杨海锋[1] 司文帅[1,2] GUO Can;WANG Shou-Ying;HUANG Zhi-Ying;BAI Bing;ZOU Yi;YANG Hai-Feng;SI Wen-Shuai(Institute for Agro-food Standards and Testing Technology of Shanghai Academy of Agricultural Sciences,Shanghai 201403,China;Shanghai Co-Elite Agri-food Testing Technical Service Co.,Ltd.,Shanghai 201403,China)

机构地区：[1]上海市农业科学院农产品质量标准与检测技术研究所,上海201403 [2]上海市科立特农产品检测技术服务有限公司,上海201403

出　　处：《食品安全质量检测学报》2024年第22期196-203,共8页Journal of Food Safety and Quality

基　　金：农业农村部行业标准制修订项目(14192063)。

摘　　要：目的建立QuEChERS-液相色谱-串联质谱法测定水产品中双甲脒及其代谢物2,4-二甲基苯胺残留量的分析方法。方法样品经磷酸氢二钠缓冲液调节pH后,经乙腈提取,盐析分层,再通过QuEChERS方法净化,供液相色谱-串联质谱仪测定,内标法定量。结果双甲脒及其代谢物的分离和洗脱在8min内完成。在1、2、10μg/kg 3个水平的加标浓度下,双甲脒的平均加标回收率为108.9%~111.1%,2,4-二甲基苯胺为100.6%~105.9%;批内RSDs为1.4%~4.5%,批间RSDs为8.0%~9.9%,4种基质的批间相对标准偏差在3.1%~11.3%之间,基质效应为–17.9%~+14.0%。方法检出限为0.5μg/kg,定量限为1.0μg/kg。结论该方法高效、准确,适用于水产品中双甲脒及其代谢物残留量的测定,并为相关标准制修订提供参考。Objective To develop an analytical method for the quantification of amitraz and its metabolite 2,4-dimethylaniline residues in aquatic products using the QuEChERS coupled with liquid chromatography-tandem mass spectrometry.Methods The samples were extracted using acetonitrile after pH adjustment with a disodium hydrogen phosphate buffer,separated by salting out,and subsequently subjected to cleanup using the QuEChERS method for determination via liquid chromatography-tandem mass spectrometry.The quantification was performed using the internal standard method.Results The separation and elution of amitraz and its metabolites were successfully accomplished within a time frame of 8 minutes.The average recoveries of dimethylamidine and 2,4-dimethylaniline were 108.9%–111.1%and 100.6%–105.9%respectively at 3 levels of 1,2,10μg/kg.Between batch RSDs of 1.4%–4.5%,within the RSDs of 8.0%-9.9%.The relative standard deviations of the four substrates ranged from 3.1%to 11.3%,and the matrix effect ranged from–17.9%-+14.0%.The limits of detection and quantitation were 0.5μg/kg and 1.0μg/kg respectively.Conclusion The proposed method demonstrates high efficiency and accuracy in the determination of amitraz and its metabolites in aquatic products,thereby offering valuable insights for the revision of relevant standards.

关 键 词：双甲脒 2 4-二甲基苯胺 液相色谱-串联质谱法 水产品 QUECHERS 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]