QuEChERS-高效液相色谱-串联质谱法测定鲤鱼和小龙虾中毒氟磷残留  

Determination of dufulin residues in carp and crayfish by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

作　　者：郑坤明 陈劲星 苏建峰 连文浩 陈冬花 张钰萍[2] 胡德禹[2] ZHENG Kunming;CHEN Jinxing;SU Jianfeng;LIAN Wenhao;CHEN Donghua;ZHANG Yuping;HU Deyu(Fujian CCIC-Faifrreach Food Safety Testing Co.,Ltd,Fuzhou 350028,China;Research and Development Center for Fine Chemicals,State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering,Key Laboratory of Green Pesticide and Agricultural Bioengineering,Ministry of Education,Guizhou University,Guiyang 550025,China)

机构地区：[1]福建中检华日食品安全检测有限公司,福州350028 [2]贵州大学精细化工研究开发中心,绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室,贵阳550025

出　　处：《农药学学报》2020年第5期909-914,共6页Chinese Journal of Pesticide Science

基　　金：国家自然科学基金(21667007).

摘　　要：建立了鲤鱼和小龙虾中毒氟磷残留的QuEChERS-高效液相色谱-串联质谱检测方法。样品经乙腈提取,采用50 mg乙二胺-N-丙基硅烷(PSA)、50 mg十八烷基键合硅胶(C18)和50 mg无水硫酸镁分散萃取净化,以Eclipse XDB-C18色谱柱分离待测物,采用电喷雾离子化正离子扫描和多反应监测模式(MRM)检测,以空白基质匹配标准溶液外标法定量。结果表明:在1.0~50μg/L范围内,毒氟磷质量浓度与相应的峰面积间呈良好线性关系,相关系数均大于0.999,其在鲤鱼和小龙虾中的检出限(LOD)分别为0.4和0.8μg/kg,定量限(LOQ)分别为2和3μg/kg;在10、50和100μg/kg添加水平下,鲤鱼和小龙虾2种基质中毒氟磷的日内和日间回收率为88%~103%,相对标准偏差(RSD)为1.2%~5.4%。该方法操作简便、经济、环保,能够满足鲤鱼和小龙虾中毒氟磷快速检测要求。A rapid method for the determination of dufulin residues in the carp and crayfish by QuEChERS-high performance liquid chromatography-tandem mass spectrometry was developed.The samples were extracted with acetonitrile,and cleaned up by 50 mg PSA,50 mg C18 and 50 mg MgSO4.The samples were separated on a Eclipse XDB-C18 column,and detected under positive polarity multiple reactions monitoring(MRM)mode.The matrix matched external standard calibration curves were used for quantitative analysis.The result indicated that the good linearities of dufulin was in the concentration range of 1.0-50μg/L with correlation coefficients higher than 0.999.At the fortified levels of 10,50 and 100μg/kg,the average recoveries of dufulin in the carp and crayfish,were in the range of88%-103%,with intra-and inter-day relative standard deviations varies from 1.2%to 5.4%.The limit of detections(LOD)for carp and crayfish were 0.4 and 0.8μg/kg,respectively.And the limit of quantifications(LOQ)of dufulin for them were 2 and 3μg/kg,respectively.This method was simple,accurate,economic and friendly to the environment,which could meet the requirements for rapid determination of dufulin residues in the carp and crayfish.

关 键 词：QUECHERS 高效液相色谱-串联质谱 鲤鱼 小龙虾 毒氟磷 残留 

分 类 号：S482.2[农业科学—农药学] TQ450.263[农业科学—植物保护]