| 焦志鹏 1, 2, 张克发 2, 潘兴鲁 2, 吴小虎 2, 徐 军 2, 郑永权 2, 董丰收 1, 2*.超高效液相色谱-串联质谱法同时检测蜜蜂中47种农药残留[J].植物保护,2026,52(4):330-340. |
| 超高效液相色谱-串联质谱法同时检测蜜蜂中47种农药残留 |
| Simultaneous determination of 47 pesticide residues in honeybees by UPLC-MS/MS |
| 投稿时间：2025-10-08 修订日期：2025-11-11 |
| DOI：10.16688/j.zwbh.2025513 |
| 中文关键词: 蜜蜂 农药残留 液相色谱串联质谱 |
| 英文关键词:honeybee pesticide residue UPLC-MS/MS |
| 基金项目:国家自然科学基金(32472620) |
| 作者 | 单位 | E-mail | | 焦志鹏 1, 2, 张克发 2, 潘兴鲁 2, 吴小虎 2, 徐 军 2, 郑永权 2, 董丰收 1, 2* | 1. 天津农学院园艺园林学院, 天津 300384
2. 中国农业科学院植物保护研究所, 植物病虫害综合治理全国重点实验室, 北京 100193 | dongfengshou@caas.cn |
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| 中文摘要: |
| 农药对蜜蜂的影响一直备受关注, 但当前的监测方法受限于样品复杂基质干扰以及农药种类覆盖有限, 难以对蜜蜂农药暴露风险进行准确评估。因此, 本研究针对蜜蜂在农业环境中可能经常接触的农药种类, 建立了QuEChERS-超高效液相色谱-串联质谱法同时检测蜜蜂中47种农药残留的分析方法, 以全面评估蜜蜂个体中的农药暴露水平, 为蜜蜂中农药残留检测提供科学的方法依据。蜜蜂样品经1%乙酸-乙腈振荡提取后, 使用几丁质净化, 流动相为乙腈和0.1%甲酸水, 采用C18色谱柱进行分离, 基质匹配标准曲线外标法定量分析。结果表明:在0.01、0.1 mg/kg和1 mg/kg 3个添加水平下, 目标化合物的平均回收率为70.6%~119.5%, 相对标准偏差(RSD)为1.1%~19.3%, 该方法在0.01~1 mg/kg范围内线性良好, 决定系数R 2≥0.99, 定量限(LOQ)为0.01 mg/kg。利用该方法对云南省红河哈尼族彝族自治州建水县某蓝莓产区和甘肃省兰州市皋兰县某温室大棚的蜜蜂样品进行测定, 发现啶酰菌胺、咯菌腈、吡唑醚菌酯、戊唑醇有检出, 残留量在<0.010~0.147 mg/kg之间, 其余43种农药残留量均低于LOQ。本研究首次将几丁质作为蜜蜂复杂基质的净化剂, 有效减少了基质干扰, 该方法准确、快速、灵敏度高, 可满足蜜蜂中47种农药的检测要求。 |
| 英文摘要: |
| The impact of pesticides on honeybees has attracted wide attention. However, current monitoring methods are limited by complex sample matrices and incomplete coverage of pesticide types, which hinders accurate assessment of pesticide exposure in honeybees. In this study, a QuEChERS-UPLC-MS/MS method was developed to simultaneously detect 47 pesticides in honeybees commonly exposed in agricultural environments. Honeybees samples were extracted with 1% acetic acid in acetonitrile and purified using chitin. Separation was performed on a C18 column with acetonitrile and 0.1% formic acid in water as the mobile phase. Quantification was conducted using an external standard calibration with matrix-matched curves. At spiking levels of 0.01, 0.1, and 1 mg/kg, recoveries of the target pesticides ranged from 70.6% to 119.5%. The relative standard deviations were between 1.1% and 19.3%. Good linearity was obtained over 0.01-1 mg/kg, with R 2≥0.99. The limit of quantification was 0.01 mg/kg. The method was applied to honeybee samples from a blueberry field in Jianshui county, Honghe Hani and Yi autonomous prefecture, Yunnan province and a greenhouse in Gaolan county, Gansu province. Boscalid, fludioxonil, pyraclostrobin, and tebuconazole were detected, with concentrations from <0.010 to 0.147 mg/kg. The other 43 pesticides were all below the LOQ. Chitin was used for the first time as a purification agent for complex honeybees matrices, effectively reducing matrix interference. This method is accurate, fast and sensitive, and it is suitable for the determination of 47 pesticides in honeybees. |
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