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高效液相色谱/串联质谱法研究溴氰菊酯在中华绒螯蟹体内的富集消除规律

Study on the accumulation and elimination of deltamethrin in Eriocheir sinensis by high performance liquid chromatography/tandem mass spectrometry

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【作者】 杨宗英房文红周俊芳胡鲲杨先乐

【Author】 YANG Zong-ying;FANG Wen-hong;ZHOU Jun-fang;HU Kun;YANG Xian-le;Key Laboratory of East China Sea & Oceanic Fishery Resources Exploitation and Utilization, Ministry of Agriculture;Nanchang Academy of Agricultural Sciences;State Collection Center of Aquatic Pathogen, Shanghai Ocean University;

【通讯作者】 胡鲲;

【机构】 农业部东海与远洋渔业资源开发利用重点实验室南昌市农业科学院上海海洋大学国家水生动物病原库

【摘要】 本研究建立了中华绒螯蟹(Eriocheir sinensis)体内溴氰菊酯残留的液相色谱/串联质谱检测方法,并选择溴氰菊酯对中华绒螯蟹的安全质量浓度0.66μg/L,在(20±1)℃下,对中华绒螯蟹进行浸浴,研究溴氰菊酯在中华绒螯蟹体内的富集消除规律。样品经乙腈提取,采用电喷雾正离子源(ESI+)和多重反应监测(MRM)模式测定,基质匹配标准曲线定量。结果表明,溴氰菊酯标准曲线在0.1~50.0μg/L质量浓度线性关系良好,决定系数为0.999 8,检测限为0.035μg/L。0.10μg/kg(μg/L)、10.00μg/kg(μg/L)、20.00μg/kg(μg/L)和50.00μg/kg(μg/L)添加水平下,溴氰菊酯回收率为82.63%~101.00%。各组织对溴氰菊酯的富集能力不同,其中血淋巴和鳃富集能力较强。血淋巴、肝胰腺和鳃等组织中药物质量浓度同时达到峰值,达到峰值时间(Tmax)为0.5 h,峰值质量浓度或质量分数(Cmax)分别为2.780μg/L,0.567μg/kg和1.165μg/kg。为了最大限度地避免溴氰菊酯残留对人体造成的危害,除了选择中华绒螯蟹重要的可食组织肝胰腺作为检测对象外,还应选择血淋巴等组织进行进一步的药残检测。

【Abstract】 A method for the determination of deltamethrin in Eriocheir sinensis by liquid chromatography/tandem mass spectrometry was established. The crabs were given a immersion bath in the safe concentration of deltamethrin at the dose of 0.66 μg/L and temperature of(20±1) ℃ to investigate the rule of accumulation and elimination of deltamethrin in E. sinensis. The samples were extracted by acetonitrile. Electrospray positive ion source(ESI+), multiple reaction monitoring mode(MRM) and matrix-matched external standard method were applied to sample analysis. Results indicated that the standard curve of deltamethrin was in good linearity in the range of 0.1-50.0 μg/L, the coefficient of determination was 0.999 8, and the detection limit was 0.035 μg/L. The recoveries for deltamethrin at the addition of 0.10 μg/kg(μg/L), 10.00 μg/kg(μg/L), 20.00 μg/kg(μg/L) and 50.00 μg/kg(μg/L) ranged from 82.63% to 101.00%. The enrichment capacities of different tissues of E. sinensis for deltamethrin were different, the capacities of hemolymph and gills were comparatively stronger. The concentrations of deltamethrin in hemolymph, hepatopancreas and gills reached their Cmax(2.780 μg/L, 0.567 μg/kg and 1.165 μg/kg) at the same time at 0.5 h(Tmax). In order to avoid the harm caused by deltamethrin residue to the human body, the hemolymph and other tissues should be also selected as the object of drug residue detection except for hepatopancreas, which is the important edible tissue of E. sinensis.

【基金】 农业部东海与远洋渔业资源开发利用重点实验室开放课题
  • 【文献出处】 江苏农业学报 ,Jiangsu Journal of Agricultural Sciences , 编辑部邮箱 ,2019年03期
  • 【分类号】TS254.7;O657.63
  • 【网络出版时间】2019-07-15 13:35
  • 【下载频次】204
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