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Determination of pesticide residues in dates using UHPLC-QqQ-MS/MS: method development and validation
Environmental Monitoring and Assessment ( IF 2.9 ) Pub Date : 2021-09-01 , DOI: 10.1007/s10661-021-09361-y
Somia Qayyum 1, 2 , Touqeer Taj 1 , Muhammad Tauseef 1 , Muhammad Ishtiaq 1 , Nazia Rafique 1 , Karam Ahad 1 , Muhammad Aslam Mirza 2 , Muhammad Aziz Choudhary 2 , Farrakh Mehboob 1
Affiliation  

A modified, efficient, and sensitive acetate-buffered QuEChERS extraction method was developed for the quantitative study of 16 commonly applied multiclass pesticides on date palm fruit. The date palm fruit samples were rehydrated by adding water during comminution. Samples were extracted with acidified acetonitrile, buffered with acetate salt. To minimize the matrix interferences, clean-up of the rehydrated samples was optimized by comparison with different sorbents (alumina, silica gel, florisil, primary secondary amine (PSA), and chitosan). The method validation parameters were evaluated as per European Union (EU) guidelines (SANTE/12682/2019). For 16 pesticides, % recovery of 69 to 121.8% with an associated precision (RSD ≤ 20%) was achieved at the fortification levels that were 0.5 to 2 times of European Union maximum residue limits (EU-MRLs). The validated method was successfully employed for the analysis of date palm fruit samples (n = 20) collected from various markets. Forty percent (40%) of samples (n = 8) were found to be contaminated with various pesticides. The most frequently detected residues were carbofuran, carbaryl, metalaxyl, tebuconazole, triazophos, and pyriproxyfen. The concentration of all the detected pesticides in real samples was below the EU-MRLs.



中文翻译:

使用 UHPLC-QqQ-MS/MS 测定枣中的农药残留:方法开发和验证

开发了一种改进的、高效且灵敏的醋酸盐缓冲 QuEChERS 提取方法,用于对枣椰果上 16 种常用的多类农药进行定量研究。通过在粉碎过程中加水使椰枣果实样品再水化。样品用酸化乙腈萃取,用醋酸盐缓冲。为了最大限度地减少基质干扰,通过与不同吸附剂(氧化铝、硅胶、氟硅酸、伯仲胺 (PSA) 和壳聚糖)进行比较,优化了再水化样品的净化。根据欧盟 (EU) 指南 (SANTE/12682/2019) 评估方法验证参数。对于 16 种农药,在欧盟最大残留限量 (EU-MRL) 的 0.5 至 2 倍的强化水平下,实现了 69% 至 121.8% 的回收率和相关精度 (RSD ≤ 20%)。n  = 20) 从各个市场收集。发现百分之四十 (40%) 的样品 ( n  = 8) 被各种农药污染。最常检测到的残留物是克百威、甲萘威、甲霜灵、戊唑醇、三唑磷和吡丙醚。实际样品中所有检测到的农药浓度均低于 EU-MRL。

更新日期:2021-09-02
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