自组装管尖固相萃取/超高效液相色谱-高分辨质谱法测定水果中的15种酸性农药  

Determination of 15 Acidic Pesticides in Fruit by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry with a Self-assembly Pipette Tip Solid-phase Extraction

作　　者：邱楠楠[1] 董桂贤[2] 陈达炜[1] 周爽[1] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室,北京100021 [2]烟台市疾病预防控制中心,山东烟台264003

出　　处：《分析测试学报》2017年第1期31-36,共6页Journal of Instrumental Analysis

基　　金：国家食品安全风险评估中心高层次人才队伍建设523项目

摘　　要：建立自组装管尖固相萃取结合超高效液相色谱-高分辨质谱检测水果中15种酸性农药残留的分析方法。水果样品经甲酸-乙腈(1∶99,体积比)提取后,以官能化聚苯乙烯/二乙烯苯(PEP)和亲水作用色谱(HILIC)作为吸附填料进行管尖固相萃取净化。以T3色谱柱进行色谱分离,采用高分辨质谱的t SIM/dd MS2扫描模式进行定性、定量分析,内标法测定。15种酸性农药在各自线性范围内呈良好的线性关系,相关系数(r2)均大于0.99。方法的定量下限(LOQ)为0.2~10μg/kg。在LOQ,10μg/kg,100μg/kg加标水平下,15种酸性农药的回收率为73.5%~115.9%,相对标准偏差为1.0%~8.3%。该方法灵敏、准确,适用于水果中酸性农药残留的分析测定,具有很好的实际应用价值。A self-assembly pipette tip solid-phase extraction（PTSPE）/high-resolution benchtop Q Exactive mass spectrometric（HRMS） method for the analysis of 15 acidic pesticides in fruit was established.The samples were first extracted with 1% formic acid in acetonitrile,and then the extracts were cleaned up using PTSPE procedure with the adsorbent of PEP and HILIC.The chromatographic analysis was performed on a T3 column.And the qualitative and quantitative analyses were performed under tSIM/ddMS2 mode by high resolution mass spectrometry.The internal standard calibration was used for quantification,and the method showed a good linearity（r2〉0.99） in a certain concentration range for the 15 acidic pesticides.The limits of quantitation（LOQ） were between 0.2μg/kg and 10μg/kg.The recoveries of the analytes in apples,cherry tomatoes and strawberries samples at spiked levels of LOQ,10μg/kg and 100μg/kg ranged from 73.5% to 115.9%,with relative standard deviations（RSDs） of 1.0%-8.3%.The results showed that the method was sensitive and accurate,and was suitable for the analysis of acidic pesticides in fruit.

关 键 词：管尖固相萃取 超高效液相色谱-高分辨质谱法 水果 酸性农药 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]