陈庭男, 齐沛沛, 华修德, 王鸣华, 何吉, 闻路红, 章文天, 王新全. 基于磁固相萃取-便携式离子阱质谱的蔬菜中3种农药残留的快速检测[J]. 农药学学报, 2023, 25(5): 1165-1172. DOI: 10.16801/j.issn.1008-7303.2023.0070
    引用本文: 陈庭男, 齐沛沛, 华修德, 王鸣华, 何吉, 闻路红, 章文天, 王新全. 基于磁固相萃取-便携式离子阱质谱的蔬菜中3种农药残留的快速检测[J]. 农药学学报, 2023, 25(5): 1165-1172. DOI: 10.16801/j.issn.1008-7303.2023.0070
    CHEN Tingnan, QI Peipei, HUA Xiude, WANG Minghua, HE Ji, WEN Luhong, ZHANG Wentian, WANG Xinquan. Rapid detection of three pesticide residues in vegetables based on magnetic solid phase extraction and portable ion trap mass spectrometer[J]. Chinese Journal of Pesticide Science, 2023, 25(5): 1165-1172. DOI: 10.16801/j.issn.1008-7303.2023.0070
    Citation: CHEN Tingnan, QI Peipei, HUA Xiude, WANG Minghua, HE Ji, WEN Luhong, ZHANG Wentian, WANG Xinquan. Rapid detection of three pesticide residues in vegetables based on magnetic solid phase extraction and portable ion trap mass spectrometer[J]. Chinese Journal of Pesticide Science, 2023, 25(5): 1165-1172. DOI: 10.16801/j.issn.1008-7303.2023.0070

    基于磁固相萃取-便携式离子阱质谱的蔬菜中3种农药残留的快速检测

    Rapid detection of three pesticide residues in vegetables based on magnetic solid phase extraction and portable ion trap mass spectrometer

    • 摘要: 针对当前我国典型的高风险蔬菜芹菜、韭菜和豇豆中易超标农药啶虫脒、吡虫啉及禁限用农药克百威的残留问题,基于磁固相萃取和便携式离子阱质谱构建了多农药残留现场、快速检测技术。系统优化了磁固相萃取方法的关键影响因素,最佳优化条件为:2 g蔬菜样品经20 mL水萃取后,采用30 mg磁固相吸附剂,超声辅助吸附水溶液中目标农药15 min,再用4 mL体积分数为0.1%的甲酸乙腈超声解吸附3 min后进行便携式质谱分析。方法验证结果表明:啶虫脒、吡虫啉及克百威3种农药在芹菜、韭菜和豇豆样品基质溶液中的线性范围为0.01~0.25 mg/L (除吡虫啉在韭菜中的线性范围为0.05~0.5 mg/L外);检出限均为0.001~0.035 mg/L,定量限均为0.02~0.05 mg/kg;在0.02、0.05和0.2 mg/kg 3个添加水平下时,3种农药的回收率在50%~71%之间,相对标准偏差在4.2%~22%之间。该方法具有较好正确度、精密度和操作便捷等优势,在蔬菜中多种农药残留的快速定性/半定量筛查方面具有广阔的应用前景。

       

      Abstract: A rapid method was established for the detection of acetamiprid, imidacloprid and carbofuran in three typically high residue vegetables, including celery, leek and cowpea, using magnetic solid-phase extraction and portable ion trap mass spectrometer. The main extraction conditions were optimized and the suitable procedures were as follows: The vegetable samples were extracted by 20 mL water, and the target pesticides in the extracted solution was then adsorbed by 30 mg magnetic solid-phase absorbents using the ultrasonic extraction for 15 min. After the magnetic separation, the adsorbed pesticides were desorbed with 4 mL of acetonitrile with 0.1% (V/V) formic acid by ultrasonic extraction for 3 min. Method validation indicated that all the three pesticides showed good linearity in the range of 0.01-0.25 mg/L, except that it was 0.05-0.5 mg/L for imidacloprid in leek sample. The limits of detection were 0.001-0.035 mg/L, and the limits of quantitation were 0.02-0.05 mg/kg. The spiked recoveries ranged from 50% to 71% with the RSDs of 4.2% to 22% at the spiked levels of 0.02, 0.05 and 0.2 mg/kg. The presented method displayed good qualitative/semi quantitative ability, and could be used for simultaneous and rapid on-site detection of multiple pesticide residues in vegetables.

       

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