蒋万枫,杨钊,张宁,张凤艳.超高效液相色谱-四级杆-飞行时间质谱法快速筛查与确证蔬菜水果中的多种农药残留[J].中国食品卫生杂志,2017,29(4):454-459. 本文二维码信息
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超高效液相色谱-四级杆-飞行时间质谱法快速筛查与确证蔬菜水果中的多种农药残留
Rapid screening and confirmation of multiple pesticide residues in vegetable and fruit by ultra performance liquid chromatography-Q-time of flight mass spectrometry
投稿时间:2017-04-25  
DOI:
中文关键词:  农药残留  水果  蔬菜  筛查  确证  超高效液相色谱  飞行时间质谱  食品污染物
Key Words:Pesticide residues  fruit  vegetable  screening  confirmation  ultra performance liquid chromatography  time of flight mass spectrometry  food contaminants
基金项目:
作者单位E-mail
蒋万枫 青岛市食品药品检验研究院,山东 青岛 266071 jwfvip@126.com 
杨钊 青岛市食品药品检验研究院,山东 青岛 266071  
张宁 青岛市食品药品检验研究院,山东 青岛 266071  
张凤艳 青岛市食品药品检验研究院,山东 青岛 266071  
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中文摘要:
      目的 应用超高效液相色谱-四极杆-飞行时间质谱技术,针对GB 2763—2014《食品安全国家标准 食品中农药最大残留限量》规定的农药残留,整合多种检测方法,建立无需标准品的快速筛查与确证蔬菜、水果中多种农药残留的方法。方法 通过一级精确质量数据库比对样品准分子离子的精确质量数、同位素分布与丰度,对蔬菜、水果中农药残留进行初筛,通过实际测定样品的二级谱图与二级谱库中谱图进行比对或通过图谱解析方法进行确证。结果 通过基质加标进行了方法验证,10.0和50.0 μg/kg添加水平检出率均为100%,90%以上的农药化合物回收率在70%~120%,并且相对标准偏差(RSD)≤20%(n=5)。对30份蔬菜、水果样品进行筛查与确证,共检出27种农药残留,并依据GB 2763—2014进行了判定,共有2份样品超标。结论 该方法的灵敏度、准确性和重复性良好,可以在较短的时间内,甚至在没有标准品的情况下,对GB 2763—2014中数百种农药进行筛查与确证,可为食品安全监管提供有效保障。
Abstract:
      Objective An analytical method for rapid screening and confirmation of multiple pesticide residues in vegetable and fruit was established according to GB 2763-2014 national food safety standard-maximum residue limits for pesticides in food, using ultra performance liquid chromatography-Q-time of flight mass spectrometry (UPLC-Q-TOF-MS). Methods Pesticide residues in vegetable and fruit were screened by comparing the accurate mass, isotope distribution and abundance in the accurate mass database, and confirmed by comparing with the spectra in the spectra library or by the spectral analysis method. Results The method was verified by spiked samples, and all pesticides were detected at the addition level of 10.0 and 50.0 μg/kg. The recovery of 90% of the pesticides was in the range of 70%-120%, with relative standard deviation (RSD) ≤20% (n=5). The method was applied to screen pesticides in 30 samples of vegetables and fruits. Twenty-seven pesticides were found and 2 samples exceeded the limit. Conclusion The method was sensitive, accurate and reproducible. Hundreds of pesticides in GB 2763-2014 could be screened and confirmed in a short period of time even without standard substance. It could provide an effective method for food safety control.
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