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QuEChERS 法和 LC-MS/MS 分析柿子小宗作物中的农药残留量,以新推导出其最大残留限量。

Analysis of Pesticide Residues by QuEChERS Method and LC-MS/MS for a New Extrapolation of Maximum Residue Levels in Persimmon Minor Crop.

机构信息

Unit of Plant Protection Products, INIA-CSIC, Ctra. La Coruña, km. 7.5, 28040 Madrid, Spain.

出版信息

Molecules. 2022 Feb 23;27(5):1517. doi: 10.3390/molecules27051517.

Abstract

According to EU guidance SANCO/7525/VI/95 Rev. 10.3, residue data extrapolation from a surrogate major crop to a minor crop can be used for setting maximum residue levels (MRLs) with a reduced number of residue trials and representative selected pesticides. In this work, a QuEChERS method (citrate-buffered version and PSA with MgSO clean-up) and LC-ESI-MS/MS for the determination of boscalid, pyraclostrobin, fludioxonil, fluopyram and tebuconazole in persimmon was developed and validated according to EU Commission guidelines and afterwards used for the determination of residues in four field trials. Residue levels at harvest for each pesticide ranged between 0.347 and 0.028 mg/kg. After comparing EFSA residue data on apples, as the surrogate major crop, and conducting a consumer risk assessment, a proposal of residue data extrapolation to set MRLs in persimmons was performed. The results showed that pesticide residues in persimmons at harvest were consistently lower than residues in apples when substances were applied according to the same critical GAP. MRLs were set at 0.5 mg/kg for fludioxonil, 0.6 mg/kg for boscalid, 0.3 mg/kg for tebuconazole, 0.4 mg/kg for fluopyran and 0.3 mg/kg for pyraclostrobin. The ratio of the MRLs for apple/persimmon varied between 2.5 for boscalid and 1.25 for fluopyram, suggesting that residue extrapolation can be feasible, promoting the process of pesticide registration for minor crops and the settlement of MRL.

摘要

根据欧盟指导方针 SANCO/7525/VI/95 Rev. 10.3,从替代主要作物向次要作物推断残留数据可用于在减少残留试验数量和代表性选择农药的情况下设定最大残留限量 (MRL)。在这项工作中,根据欧盟委员会指南开发并验证了用于测定柿子中 boscalid、pyraclostrobin、fludioxonil、fluopyram 和 tebuconazole 的 QuEChERS 方法(柠檬酸盐缓冲版本和 PSA 与 MgSO4 净化)和 LC-ESI-MS/MS,随后用于在四项田间试验中测定残留量。每种农药在收获时的残留水平在 0.347 至 0.028 mg/kg 之间。在比较 EFSA 在苹果(作为替代主要作物)上的残留数据并进行消费者风险评估后,提出了将残留数据推断用于设定柿子中 MRL 的建议。结果表明,当按照相同的关键 GAP 施用物质时,柿子在收获时的农药残留始终低于苹果中的残留。将 fludioxonil 的 MRL 设定为 0.5 mg/kg,boscalid 的 MRL 设定为 0.6 mg/kg,tebuconazole 的 MRL 设定为 0.3 mg/kg,fluopyram 的 MRL 设定为 0.4 mg/kg,pyraclostrobin 的 MRL 设定为 0.3 mg/kg。苹果/柿子的 MRL 比值在 boscalid 为 2.5,fluopyram 为 1.25 之间变化,表明残留推断是可行的,这促进了次要作物的农药登记过程和 MRL 的确定。

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