| 朱 峰1, 龙育鋆1, 宋邦燕1, 张海艳1, 廖国会1, 陈明贵1, 陈湘燕1, 秦立新1, 马玉华2*.QuEChERS-UPLC-MS/MS法同时检测李子中29种农药残留[J].植物保护,2025,51(1):181-189. |
| QuEChERS-UPLC-MS/MS法同时检测李子中29种农药残留 |
| Simultaneous determination of 29 pesticides residues in plums by QuEChERS-UPLC-MS/MS |
| 投稿时间：2024-01-26 修订日期：2024-03-21 |
| DOI：10.16688/j.zwbh.2024052 |
| 中文关键词: 农药 残留 李子 QuEChERS 超高效液相色谱串联质谱 |
| 英文关键词:pesticides residue plum QuEChERS UPLC-MS/MS |
| 基金项目:贵州省优秀青年科技人才计划(黔科合平台人才(YQK[2023]026)); 贵州省农业科学院博士基金(黔农科博士基金[2024]07号) |
| 作者 | 单位 | E-mail | | 朱 峰1, 龙育鋆1, 宋邦燕1, 张海艳1, 廖国会1, 陈明贵1, 陈湘燕1, 秦立新1, 马玉华2* | 1. 贵州省农业科学院植物保护研究所(贵州省农药风险监测中心), 贵阳 550006
2. 贵州省农业科学院, 贵阳 550006 | m_yh79@163.com |
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| 中文摘要: |
| 本研究建立了基于QuEChERS前处理方法同时检测李子果实中29种农药残留的超高效液相色谱串联质谱(UPLC-MS/MS)分析方法?样品经1%乙酸-乙腈提取, 50 mg PSA和30 mg GCB净化后采用UPLC-MS/MS检测, 以0.5 mmol/L乙酸铵-0.1%甲酸水为水相, 乙腈为有机相进行梯度洗脱, 基质外标法定量?29种农药在0.001~0.1 mg/kg范围内呈良好的线性关系, 决定系数(R2)大于0.990; 在0.001?0.01?0.1 mg/kg 3个添加水平下, 29种农药在李子中的平均添加回收率为70.6%~114.0%, 相对标准偏差为1.0%~9.7% (n=5)?29种农药的定量限为0.001 mg/kg?采用所建立的方法对贵州省10批李子样品进行残留检测, 结果显示, 李子中共检出18种农药, 残留量均小于0.104 7 mg/kg?该方法的精密度和灵敏度均满足农药残留检测分析要求, 能简单?快速地同时检测李子中29种农药残留? |
| 英文摘要: |
| This study established a method for the simultaneous analysis of 29 pesticides residues in plums using QuEChERS-based ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS/MS). The samples were extracted with acetonitrile containing 1% acetic acid, purified with 50 mg PSA and 30 mg GCB, and detected by UPLC-MS/MS. Gradient elution was performed using 0.5 mmol/L ammonium acetate and 0.1% formic acid in water as the aqueous phase, and acetonitrile as the organic phase, with external matrix standard quantification. The 29 pesticides showed a good linear relationship in the range of 0.001-0.1 mg/kg, with determination coefficients (R2) greater than 0.990. The average recoveries of the 29 pesticides ranged from 70.6% to 114.0%, with relative standard deviation (RSD) of 1.0%-9.7% (n=5) at spiking levels of 0.001 mg/kg, 0.01 mg/kg, and 0.1 mg/kg. The limits of quantification (LOQ) for the 29 pesticides were 0.001 mg/kg. Residue analysis of 10 batches of plum samples from Guizhou province showed that a total of 18 pesticides were detected, with the residue level lower than 0.104 7 mg/kg. The precision and sensitivity of this method meet the requirements for pesticide residue detection, providing a simple and rapid approach for simultaneous detection of 29 pesticide residues in plums. |
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