凝胶渗透色谱净化气相色谱-三重串联四极杆.pdf

凝胶渗透色谱净化气相色谱-三重串联四极杆质谱联用测定食用油中的腐霉利残留 廖且根，罗林广∗，陆彦锋∗ (江西省农业科学院农产品质量安全与标准研究所，江西省农业科学院农产品质量安全重点 实验室，南昌，330200) 摘要：为了快速检测和确证食用油中的腐霉利残留量，建立了气相色谱-三重串联四极杆质 谱联用法（GC-MS/MS ）测定食用油中的腐霉利残留分析方法。样品用（V/V=1/1 ）环己烷/ 乙酸乙酯溶解，凝胶渗透色谱（GPC ）净化浓缩后，采用GC-MS/MS 多反应监测模式(MRM) 检测，外标法定量。腐霉利为 1.0-200.0 μg/l 浓度范围内与其峰面积呈线性关系，其相关系 数（R ）为0.9999 。在食用油中的腐霉利残留检限为5.0 μg/kg，添加回收率在为 75.6 ％～105.7 ％之间。 关键词：气相色谱-三重串联四极杆质谱法；凝胶渗透色谱；腐霉利；食用油 Determination of by gel permeation chromatography and gas chromatography - triple quadrupole mass spectrometry * Liao Qie gen, Luo linguang (Agricultural Product Quality Safety and Standards Institute，Key Laboratory of Quality and Safety of Agricultural Products, Jiangxi Academy of Agricultural Sciences, Nanchang, 330200) Abstract: For validation and fast determination of procymidone residues in the edible oil ，the residual method was established to determinate procymidone in the edible oil by gas chromatography - triple quadrupole mass spectrometry (GC-MS ／MS) ．the edible oil was dissolved by cyclohexane and ethyl acetate(V/V=1/1) ， cleaned up by gel permeation chromatography ．Identification was carried out by GC-MS/MS in multiple reaction monitoring (MRM) mode ．There was well linear relationship between the peak area and concentration of procymidone in the range from 1.0μg /l to 200.0 μg /l, and the correlation coefficient (R) was 0.9999. The limit of detection of procymidone in the edible oi was 5.0 μ g/kg ，and the recoveries of procymidone in the edible oi were 75.6 ％-105.7 ％ Key words: Gas chromatography - triple quadrupole mass spectrometry (GC-MS/MS); Gel permeation chromatography(GPC); Procymidone; Edible oil 1 引言 腐