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作 者:陈达炜[1] 高洁[1] 吕冰[1] 朱盼[1] 杨欣[1] 赵云峰[1] 苗虹[1]
机构地区:[1]卫生部食品安全风险评估重点实验室,国家食品安全风险评估中心,北京100021
出 处:《分析化学》2014年第4期579-584,共6页Chinese Journal of Analytical Chemistry
基 金:“十二五”国家科技支撑计划(No.2011BAK10B06)资助~~
摘 要:采用超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术(UPLC/Q Orbitrap),建立土豆中农药多残留的快速筛查方法.样品采用乙腈为提取溶剂,PSA分散固相萃取净化.以BEH C18色谱柱进行色谱分离,通过静电场轨道阱质谱全扫描获得农药的精确质量数,以Full Scan/ddMS2进行定性筛查和定量检测.对欧盟考核样品土豆中175种农药残留进行分析,共从考核样品中定性筛查出17种农药残留.17种农药的高分辨质谱分析方法定量限为1 ~5 μg/kg,在1~250 μg/L的浓度范围内均呈良好的线性关系(R2>0.99);平均加标回收率为83.1%~ 115.5%,相对标准偏差在1.5%~11.8%之间.定量测定17种农药的含量范围在0.002~1.714 mg/kg之间,z评分在-1.00~ 1.24之间.本方法简单精确,灵敏度高,样品处理快捷简便,适用于农产品中农药多残留的快速筛查.Abstract A method was established for the rapid screening and confirmation of pesticide residues in potato by UPLC/Q Orbitrap. The pesticide residues were extracted from the samples with acetonitrile, and purified by dispersion solid phase extraction using PSA. The analytes were then separated on a reversed phase column ( BEH CIs, 100 mm x 2.1 mm, 1.7 ~m) using a gradient elution program. The accurate mass measurements of analytes were obtained using full scan mode by Q Exactive. In checking potato sample, 17 pesticide analytes were screened qualitatively and carried on the quantitative analysis by full scan/ddMS2 mode. The method showed a good linearity (R2 〉0.99) in the ranges of 1-250 μg/L for with average recovery rates of 83.1%-115.5% and relative standard deviation (RSD) of 1.5%-11. 8%. The limits of quantification (LOQ) were 1-5 p.g/kg. The method was simple, sensitive and accurate, and suitable for the rapid screening and confirmation of multi-residue pesticides in agricultural products.
关 键 词:四极杆-静电场轨道阱高分辨质谱仪 农药残留 土豆
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