| 夏北齐1, 2, 李如男2, 董丰收2, 郑永权1, 张清明1, 李远播2*.超高效液相色谱-串联质谱法同时测定16种农药在玉米吐水中的残留[J].植物保护,2025,51(2):193-201. |
| 超高效液相色谱-串联质谱法同时测定16种农药在玉米吐水中的残留 |
| Determination of 16 pesticide residues in maize guttation by ultra-performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2024-03-21 修订日期：2024-04-23 |
| DOI：10.16688/j.zwbh.2024161 |
| 中文关键词: 玉米 吐水 农药残留 超高效液相色谱-串联质谱 |
| 英文关键词:maize guttation pesticide residue ultra-performance liquid chromatography-tandem mass spectrometry |
| 基金项目:国家自然科学基金(32372608) |
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| 摘要点击次数: 82 |
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| 中文摘要: |
| 本研究基于改进的QuEChERS前处理方法和超高效液相色谱-串联质谱法, 建立了16种不同理化性质的农药在玉米吐水中的残留分析方法。利用乙腈提取玉米吐水样品, 经ACQUITY UPLCTMBEH C18色谱柱分离后用多反应监测模式进行定量分析, 最后通过外标法进行定量。结果表明:在0.1~1 000 μg/L范围内, 16种供试农药的质量浓度与对应的峰面积间均呈现良好线性关系, 决定系数R2≥0.997 1; 定量限(limit of quantitation, LOQ)为0.1~0.7 μg/L; 在10、100 μg/L和1 000 μg/L的3个添加浓度水平条件下, 供试农药平均回收率均在77.3%~107.4%之间, 相对标准偏差(relative standard deviations, RSD)为1.7%~13.5%。运用该方法对玉米吐水样品进行实测, 16种农药均可被检测出, 其中啶虫脒的检出浓度最高(548.8 μg/L)。该方法适用于玉米吐水中多种农药残留的同时检测。 |
| 英文摘要: |
| A method for analyzing pesticide residue of 16 pesticides with different physicochemical property in maize guttation was established based on a modified QuEChERS pretreatment method and ultra-performance liquid chromatography-tandem mass spectrometry. The maize guttation samples were extracted using acetonitrile, separated by an ACQUITY UPLCTMBEH C18 column, and quantified using multiple reaction monitoring mode, with external standard calibration for quantification. The results showed that there was a good linear relationship between the mass concentration of 16 tested pesticides and the corresponding peak area in the range of 0.1-1 000 μg/L, and the correlation coefficient was greater than 0.997 1. The limit of quantitation (LOQ) was 0.1-0.7 μg/L. The average recovery of tested pesticides ranged from 77.3% to 107.4% at three levels of 10, 100, 1 000 μg/L. The relative standard deviations (RSD) were in the range of 1.7% to 13.5%. The method was applied to detect 16 pesticides in maize guttation samples, and all the 16 pesticides could be detected. Among them, acetamiprid exhibited the highest concentration at 548.8 μg/L. This method is suitable for simultaneous detection of many pesticide residues in maize guttation. |
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