王子剑, 赵劲松, 郭晓宇, 李倩, 郑天驰, 商爱媛, 范赛. 滤过型萃取柱-超高效液相色谱-串联质谱法同时测定水果中11种农药残留[J]. 分析测试技术与仪器, 2023, 29(1): 23-29. DOI: 10.16495/j.1006-3757.2023.01.004
引用本文: 王子剑, 赵劲松, 郭晓宇, 李倩, 郑天驰, 商爱媛, 范赛. 滤过型萃取柱-超高效液相色谱-串联质谱法同时测定水果中11种农药残留[J]. 分析测试技术与仪器, 2023, 29(1): 23-29. DOI: 10.16495/j.1006-3757.2023.01.004
WANG ZiJian, ZHAO Jingsong, GUO Xiaoyu, LI Qian, ZHENG Tianchi, SHANG Aiyuan, FAN Sai. Simultaneous Determination of 11 Pesticide Residues in Fruits by Filtered Extraction Column-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 23-29. DOI: 10.16495/j.1006-3757.2023.01.004
Citation: WANG ZiJian, ZHAO Jingsong, GUO Xiaoyu, LI Qian, ZHENG Tianchi, SHANG Aiyuan, FAN Sai. Simultaneous Determination of 11 Pesticide Residues in Fruits by Filtered Extraction Column-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 23-29. DOI: 10.16495/j.1006-3757.2023.01.004

滤过型萃取柱-超高效液相色谱-串联质谱法同时测定水果中11种农药残留

Simultaneous Determination of 11 Pesticide Residues in Fruits by Filtered Extraction Column-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了超高效液相色谱-串联质谱测定水果中杀虫剂、杀菌剂、除草剂等11种常见农药的方法. 水果样品经乙腈提取,提取液经滤过型萃取柱(m-PFC)净化,正离子多反应模式(MRM)监测,外标法定量. 水果中11种农药的检出限为1~3 μg/kg,在1.0~100.0 ng/mL的范围内线性关系良好,相关系数r不低于0.996 9. 在样品基质中分别添加5、20、50 μg/kg的标准品进行加标回收试验,11种农药的平均回收率为88.9%~110.1%,相对标准偏差(RSD)为2.7%~8.5%(n=6). 方法操作简单、灵敏度高,能够准确测定水果中11种农药残留.

     

    Abstract: A method for the determination of 11 common pesticides in fruits, such as pesticides, fungicides and herbicides, was set up using the ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The fruit samples were extracted with acetonitrile, and the extracts were purified using a filtered extraction column (m-PFC), monitored by the positive ion multiple reaction mode (MRM), and quantified by the external standard method. The detection limits of 11 pesticides in fruits were 1~3 μg/kg, with good linearity in the range of 1.0~100.0 ng/mL, with the correlation coefficient r not less than 0.996 9. The standards of 5, 20 and 50 μg/kg were added to the sample matrix for spiked recovery tests. The average recoveries rate of 11 pesticides were 88.9%~110.1%, and the relative standard deviation (RSD) were 2.7%~8.5% (n=6). The method is simple and sensitive, and can accurately determine 11 pesticide residues in fruits.

     

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