仝凯旋, 盖丽娟, 霍思宇, 谢瑜杰, 吴兴强, 范春林, 陈辉, 吕美玲. 液相色谱-四极杆飞行时间质谱快速筛查洋葱中173种农药残留[J]. 农药学学报, 2023, 25(1): 210-219. DOI: 10.16801/j.issn.1008-7303.2022.0085
    引用本文: 仝凯旋, 盖丽娟, 霍思宇, 谢瑜杰, 吴兴强, 范春林, 陈辉, 吕美玲. 液相色谱-四极杆飞行时间质谱快速筛查洋葱中173种农药残留[J]. 农药学学报, 2023, 25(1): 210-219. DOI: 10.16801/j.issn.1008-7303.2022.0085
    TONG Kaixuan, GE Lijuan, HUO Siyu, XIE Yujie, WU Xingqiang, FAN Chunlin, CHEN Hui, LYU Meiling. Rapid screening of 173 pesticide residues in onion by liquid chromatography-quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Pesticide Science, 2023, 25(1): 210-219. DOI: 10.16801/j.issn.1008-7303.2022.0085
    Citation: TONG Kaixuan, GE Lijuan, HUO Siyu, XIE Yujie, WU Xingqiang, FAN Chunlin, CHEN Hui, LYU Meiling. Rapid screening of 173 pesticide residues in onion by liquid chromatography-quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Pesticide Science, 2023, 25(1): 210-219. DOI: 10.16801/j.issn.1008-7303.2022.0085

    液相色谱-四极杆飞行时间质谱快速筛查洋葱中173种农药残留

    Rapid screening of 173 pesticide residues in onion by liquid chromatography-quadrupole time-of-flight mass spectrometry

    • 摘要: 应用液相色谱-四级杆飞行时间质谱(LC-QTOF/MS)建立了洋葱中173种农药的快速筛查方法。洋葱样品经含体积分数1%乙酸的乙腈溶液振荡提取,盐析离心,Carbon/NH2净化,在电喷雾全离子二级质谱扫描 (All Ions MS/MS) 正离子模式下采用LC-QTOF/MS进行检测。选择定性筛查时较为重要的离子个数选择模式,色谱共流出曲线相似度匹配得分 (co-elution score) 以及峰高阈值等参数进行了定性筛查方法的优化,最终确定了对采集结果进行分析的最佳筛查参数。同时,应用该方法对洋葱基质中173种农药的定性和定量方法学参数进行了考察。结果表明:167种农药的筛查限和定量限分别在0.001~0.005 mg/kg和0.001~0.01 mg/kg之间,其余6种的筛查限和定量限分别在0.01~0.025 mg/kg和 0.02~0.05 mg/kg之间。所有化合物在测试浓度范围内线性关系良好。添加回收试验 (n=5) 结果显示,在1倍定量限(LOQ)、2倍LOQ和10倍LOQ 3个添加水平下,173种农药中分别有153、168和165种农药的平均回收率在70%~120%之间,相对标准偏差均在20%以内。将本研究建立的筛查方法应用于2020年欧盟组织的水果蔬菜中农药残留检测能力验证 (EUPT-FV22),准确筛查出了组织方在洋葱样品中添加的农药,而且定量结果满意,表明本研究所建立的LC-QTOF/MS筛查方法准确、可靠,适用于洋葱中农药多残留快速筛查和准确定量。

       

      Abstract: A rapid screening method for 173 pesticides in onion was established using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF/MS). Onion samples were extracted with 1% acetic acid in acetonitrile, salted out, shaken and centrifuged, then cleaned-up by SPE column with Carb/NH2. The LC-QTOF/MS detection was operated in the positive ion all ions MS/MS scanning mode of electrospray ionization. The important parameters such as maximum number of characteristic ions, co-elution score and peak height threshold were optimized for the qualitative screening, and the final screening parameters were determined for analysis of the collected results. Meanwhile, the methodological parameters of 173 pesticides in onion were investigated. The results showed that the SDL and LOQ of 167 pesticides were 0.001-0.005 mg/kg and 0.001-0.01 mg/kg, respectively, and it was 0.01-0.025 mg/kg and 0.02-0.05 mg/kg for the remaining 6 pesticides. These pesticides had good linear relationship in the test concentration range. The results of the recovery experiments showed that the average recoveries (n=5) of 153, 168 and 165 pesticides at three different levels (1 × LOQ, 2 × LOQ, 10 × LOQ) were in the range of 70%-120%, respectively, and the RSDs were all within 20%. The established screening method was applied to the proficiency test of pesticide residues in fruits and vegetables organized by the European Union in 2020 (EUPT-FV22). The pesticides spiked in onion were accurately screened, and the quantitative results were satisfactory. The results show that the LC-QTOF/MS screening method established in this work is accurate and reliable, and is suitable for rapid screening and accurate quantification of multi-pesticide residues in onion.

       

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