LC-TOF/MS无标准品定性筛查水果蔬菜中210种农药残留  

Screening 210 pesticides without reference standards in fruits and vegetables by liquid chromatography coupled time-of-flight mass spectrometry

作　　者：彭兴[1,2] 赵志远[2,3] 康健[2,4] 王志斌[2,4] 常巧英[2] 范春林[2] 庞国芳[2] 吕美玲[5] 

机构地区：[1]北京工商大学食品学院,北京100048 [2]中国检验检疫科学研究院,北京100123 [3]河北大学化学与环境科学学院,保定071002 [4]燕山大学环境与化学工程学院,秦皇岛066004 [5]安捷伦科技公司,北京100102

出　　处：《分析试验室》2014年第3期282-291,共10页Chinese Journal of Analysis Laboratory

基　　金："十二五"国家科技支撑项目(2012BAD29B01)资助

摘　　要：建立了基于农药化合物列表(Database)无需标准品定性筛查水果蔬菜中210种农药的LC-TOF/MS方法。农药化合物列表包含农药的名称、保留时间、分子式和精确质量数。实验对检索中所需的精确质量数、保留时间窗口和离子化形式等进行了对比优化,用以提高筛查准确度,避免假阳性和假阴性结果的产生。采用标准溶液和基质添加样品,对方法的准确性、稳定性以及检测能力进行了探讨,结果表明,所有农药均能在10.0μg/kg(一律标准)下检出,化合物检索得分的相对标准偏差(RSD)均<20%。只需通过1次样品前处理,1次仪器测定,借助农药化合物列表实现无标准品对照下,对210种农药进行快速定性筛查,并且其性能指标均能够满足日常检测的需要。采用本方法对20个市售水果蔬菜样品进行了测定,发现了16种农药残留,包括常用农药,如多菌灵、烯酰吗啉、啶虫脒、甲霜灵、莠去津和噻菌灵等。A novel method for determination of 210 multi-class pesticides without reference standards in fruits and vegetables by high performance liquid chromatography coupled time-of-flight mass spectrometry （HPLC-Q- TOF/MS） is established. Accurate mass database include compound name, retention time, formula, accurate mass. The parameters （accurate mass tolerance, retention time window, the ionization forms, etc. ） in the process of search were optimized to improve the screening capacity and avoid the false positive or false negative results. Standard solutions and spiked samples are applied to evaluation of the reliability, stability and capability of accurate mass database. The results indicate that all pesticides can be detected at the level of 10. 0 μg/kg （ Uniform limit） , and the RSD of search score of all compounds are lower than 20.0%. This method is simple, fast, and accurate, and only needs one time sample preparation and one times determination, based on the accurate mass database to achieve simultaneous screening 210 pesticides without reference standards, and the performance of method can meet the need of routine determination. Finally, this method has been applied to screening the pesticide residues in 20 fruit and vegetable samples （apple, cabbage, tomato, pear, peach, watermelon, cabbage, celery, cucumber, leek, pepper, courgettes, pumpkins, eggplant ） markets, 16 pesticide residues are found in these samples, such as carbendazim, dimeth metalaxyl, atrazine and thiabendazole, etc. purchased from local omorph, acetamiprid,

关 键 词：农药多残留 水果蔬菜 QUECHERS LC-TOF MS 

分 类 号：O657.63[理学—分析化学]