气相色谱-四极杆-飞行时间质谱和气相色谱-串联质谱对水果、蔬菜中208种农药残留筛查确证能力的对比  

Comparison of the performances of gas chromatographyquadrupole time of flight mass spectrometry and gas chromatography-tandem mass spectrometry in rapid screening and confirmation of 208pesticide residues in fruits and vegetables

作　　者：曹新悦[1,2] 庞国芳[2] 金铃和 康健[2,3] 胡雪艳[2] 常巧英[2,3] 王明林[1] 范春林[2] 

机构地区：[1]山东农业大学食品科学与工程学院,山东泰安271018 [2]中国检验检疫科学研究院,北京100123 [3]燕山大学环境与化学工程学院,河北秦皇岛066004

出　　处：《色谱》2015年第4期389-396,共8页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑项目(2012BAD29B01)

摘　　要：对比研究了气相色谱.串联质谱（ GC.MS／MS）与气相色谱.四极杆.飞行时间质谱（ GC.QTOF／MS）在水果、蔬菜中208种农药多残留检测中基质效应及方法学效能的差异，提出两种仪器在农药残留检测方面的特点和适用范围，为残留检测分析提供参考。在苹果、柑橘、番茄、黄瓜4种基质，3个添加浓度（5.0、10.0和20.0μg／kg）下，两种仪器中均有93.0％以上的农药回收率在70％～120％范围内且相对标准偏差（ RSD）≤20％（ n＝5）。检测灵敏度方面，绝大部分农药在两种仪器的检出限均低于5.0μg／kg，满足各国农药残留限量的要求，且GC.MS／MS灵敏度更高，线性范围更宽，定量能力更加准确。筛查确证方面，GC.QTOF／MS在快速、高通量筛查、准确定性及非目标化合物鉴定等方面表现出了优势。The performances of gas chromatography.tandem mass spectrometry （ GC.MS/MS） and gas chromatography quadrupole time of flight mass spectrometry （ GC.QTOF/MS） for the determination of 208 pesticide residues in fruit and vegetable samples, including apple, orange, tomato and cucumber, were compared comprehensively. Based on the differences of the two instruments, their respective characteristics and scopes of application in the detection of the pesticide residues were presented, which provided the reference for the analysis of pesticide residues. The performance parameters of the two instruments, such as overall recoveries, pre.cisions, limits of detection, linear ranges, identification points and matrix effects, were evalua.ted according to a designed experiment. At three spiked levels （5.0, 10.0 and 20.0 μg/kg）, the average recoveries for the majority of pesticides （ 93.0%） ranged from 70% to 120% in the four matrices with relative standard deviations below 20%. The limits of detection for most of＆amp;nbsp;the pesticides by GC.MS/MS and GC.Q.TOF/MS were less than 5.0μg/kg. Compared with GC.QTOF/MS, GC.MS/MS showed relatively lower limits of detection and wider linear ranges, and its performance was more satisfactory in accurate quantitative analysis due to its superior sensi.tivity. On the other hand, GC.QTOF/MS provided accurate mass measurement, which was proved to be an efficient analytical tool on the rapid screening and confirmation of a large num.ber of pesticides and non.target compounds.

关 键 词：气相色谱-四极杆-飞行时间质谱 气相色谱-串联质谱 农药多残留 水果蔬菜 对比 

分 类 号：O658[理学—分析化学]