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液相色谱-串联质谱法测定果蔬中4种新型卵菌纲杀菌剂残留

Determination of New Type of 4 Bactericids Used for Control of Oomycete Diseases Residues in Fruits and Vegetables by Liquid Chromatography/Tandem Mass Spectrometry

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【作者】 崔淑华许美玲钱家亮段浩刘金峰林黎明王开运

【Author】 CUI Shu-Hua1,2,XU Mei-Ling2,QIAN Jia-Liang2,DUAN Hao2, LIU Jing-Feng2,LIN Li-Ming3,WANG Kai-Yun1 1(College of Plant Protection,Shandong Agriculture University,Taian 271018) 2(Inspection and Quarantine Technology Center of Linyi Exit/Entry Inspection and Quarantine Bureau,Linyi 276034) 3(Shangdong Inspection Quarantine and Sdence Technology Academy,Qingdao 266002)

【机构】 山东农业大学植物保护学院临沂出入境检验检疫局检验检疫技术中心山东省检验检疫局科学技术研究院

【摘要】 建立了蔬菜和水果中噻唑菌胺、苯噻菌胺、氟啶酰菌胺和双炔酰菌胺4种新型卵菌纲杀菌剂的分散固相萃取-液相色谱-串联质谱检测方法。样品经乙腈均质提取,混合使用乙二胺-N-丙基硅烷(PSA)和ODSC18-N两种基质分散净化剂净化,采用液相色谱-三重四级杆串联质谱(LC/MS/MS)检测。实验通过空白基质溶液稀释标准建立校正的标准曲线,以消除基质效应。结果表明,噻唑菌胺和氟啶酰菌胺在1~100μg/L,苯噻菌胺和双炔酰菌胺在0.5~50μg/L线性范围内具有良好的线性关系,相关系数为0.9994~0.9999;4种卵菌纲杀菌剂添加回收率在80.9%~101.3%之间;相对标准偏差(RSD)均小于6.3%。定量限在0.53~1.3μg/kg之间,检出限为0.16~0.40μg/kg。

【Abstract】 A method was developed for the determination of ethaboxam,benthivalicarb-isopropyl,fluopicolide and mandipropamid in fruits and vegetables.The analytes were extracted from the samples by acetonitrile,and purified by dispersion solid phase extraction using ODS C18-N and PSA as solidphase,and then analyzed by LC/MS/MS with multiple reaction monitoring(MRM).The interference of matrix was reduced by the matrix-matched calibration standards curve.The linear range was from 1 μ /L to 100 μ /L for ethaboxam,fluopicolide,from 0.5 μ/L to 50 μ g/L for benthivalicarb-isopropyl,mandipropamid(r≥0.9994).The fortified recoveries were from 80.9% to 101.3% with relative standard deviations(RSD) lass than 6.3%.The limits of quantification were 0.53 μ g/kg to 1.3 μ g/kg and the limit of detection were 0.16 to 0.40 μ g/kg.

【基金】 国家质检公益性行业科研专项(No.200910145-2)资助
  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2011年12期
  • 【分类号】TS255.7;TS255.7
  • 【被引频次】16
  • 【下载频次】370
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