| 原海越,史小萌,李备,王雯雯,刘潇威,贺泽英.UHPLC-MS/MS和GC-MS/MS测定甜菜中523种农药及代谢物的残留量[J].农业环境科学学报,2023,42(7):1666-1674. |
| UHPLC-MS/MS和GC-MS/MS测定甜菜中523种农药及代谢物的残留量 |
| Simultaneous determination of 523 pesticides and metabolites in beet using UHPLC-MS/MS and GC-MS/MS |
| 投稿时间：2022-12-08 |
| DOI：10.11654/jaes.2022-1259 |
| 中文关键词: 甜菜 农药多残留分析 超高效液相色谱串联质谱 气相色谱串联质谱 |
| 英文关键词: beet pesticide multi-residue analysis UHPLC-MS/MS GC-MS/MS |
| 基金项目:国家市场监管重点实验室（热带果蔬质量与安全）基础应用研究课题（KF-2022009） |
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| 中文摘要: |
| 建立同时检测甜菜中523种农药及代谢物的QuEChERS提取结合超高效液相色谱串联质谱法和气相色谱串联质谱分析方法。采用 QuEChERS 前处理方法提取，MgSO4和乙二胺-N-丙基硅烷化硅胶（PSA）净化，采用 UHPLC-MS/MS 和 GC-MS/MS 检测。PSA的用量会影响 40种农药的回收率，用量为 0或 5 mg·mL-1时，回收率在 60%~120% 之间。523种农药在 2~200 μg·kg-1添加浓度水平回收率在65.1%~116.4%之间，RSD值小于24.1%。方法定量为2 μg·kg-1或5 μg·kg-1，线性相关系数均大于0.99，采用基质标准曲线定量分析。针对142种农药适用于两种仪器的检测结果无明显差异。实际样品检测出的农药残留物浓度均低于我国规定相应的最大残留限量，但根据欧盟标准的规定，部分样品中毒死蜱、溴氰菊酯和氰戊菊酯存在超标现象。该方法样品前处理简单快速，方法的准确度、精密度和灵敏度均满足农药残留在农作物中检测分析要求，适用于523种农药及代谢物在甜菜中的多残留检测。 |
| 英文摘要: |
| This study aimed to develop a multiresidue method for simultaneous detection of 523 pesticides and metabolites in beet using QuEChERS extraction combined with UHPLC-MS / MS and GC-MS / MS. The samples were extracted by the QuEChERS pretreatment method, purified by d-SPE with MgSO4 and PSA, and determined using UHPLC-MS/MS and GC-MS/MS. The dosage of PSA affected the recoveries of 40 pesticides, which were between 60% and 120% when PSA was used 0 mg ·mL-1 or 5 mg ·mL-1. The recoveries of 523 pesticides and metabolites at 2-200 μg·kg-1 ranged from 65.1% to 116.4% with RSDs <24.1%. The limits of quantification（LOQs）were 2 μg·kg-1 or 5 μg·kg-1. The linear correlation coefficients were >0.99. There was no significant difference in the detection results of the two instruments for 142 pesticides. The concentrations of pesticide residues detected in real samples were all below the corresponding national maximum residue limits（MRL）. However, according to the European Union standard, residual concentrations of chlorpyrifos, deltamethrin, and fenvalerate exceeded the MRLs in some samples. This analytical method is simple and rapid, and its accuracy, precision, and sensitivity all meet the requirements of pesticide residues analysis. Therefore, this method can be applied in analysis of 523 pesticides and metabolites in beet. |
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