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Determination of pesticide residues in dates using UHPLC-QqQ-MS/MS: method development and validation

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Abstract

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.

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Funding

This work was financially supported by Government of Pakistan under the PSDP project (PSDP-714) entitled “National Pesticides Residue Monitoring System in Pakistan (NPRMS).”

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Authors and Affiliations

  1. Ecotoxicology Research Program (ERP), National Agricultural Research Center (NARC), Islamabad, 44000, Pakistan

    Somia Qayyum, Touqeer Taj, Muhammad Tauseef, Muhammad Ishtiaq, Nazia Rafique, Karam Ahad & Farrakh Mehboob

  2. Department of Chemistry, Mirpur University of Science and Technology (MUST), Mirpur, 10250, AJ&K, Pakistan

    Somia Qayyum, Muhammad Aslam Mirza & Muhammad Aziz Choudhary

Authors
  1. Somia Qayyum
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  2. Touqeer Taj
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  3. Muhammad Tauseef
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  4. Muhammad Ishtiaq
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  5. Nazia Rafique
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  6. Karam Ahad
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  7. Muhammad Aslam Mirza
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  8. Muhammad Aziz Choudhary
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  9. Farrakh Mehboob
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Contributions

All authors contributed to the study conception and design. Conceptualization: Somia Qayyum and Farrakh Mehboob. Methodology: Somia Qayyum, Touqeer Taj, and Muhammad Tauseef. Data acquisition and analysis: Somia Qayyum, Nazia Rafique, and Muhammad Ishtiaq. Writing—original draft preparation: Somia Qayyum. Writing—review and editing: Somia Qayyum, Farrakh Mehboob, Muhammad A. Mirza, and Muhammad A. Choudhary. Supervision: Karam Ahad and Farrakh Mehboob.

Corresponding author

Correspondence to Farrakh Mehboob.

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Qayyum, S., Taj, T., Tauseef, M. et al. Determination of pesticide residues in dates using UHPLC-QqQ-MS/MS: method development and validation. Environ Monit Assess 193, 613 (2021). https://doi.org/10.1007/s10661-021-09361-y

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