Abstract
Pesticide residues in foodstuffs can lead to several undesirable effects. A simple and high-throughput targeted screening method analyzing multi-residue pesticide in aquaculture water based on ultra-high-performance liquid chromatography-Q/Orbitrap mass spectrometry (UHPLC-Q/Orbi MS) was developed and validated. In this technique, the peaks of the compound using precursor ions were recorded by the full scan, which was used for rough quantitative analysis with single point matrix matched calibration. The qualitative identification was performed following the stringent confirmation criteria with fragment ions, retention time, and an isotopic pattern. Additionally, solid-phase extraction with an HLB (Hydrophilic/Lipophilic Balanced) column was selected to enrich and separate target pesticides from water. The screening detection limit of 33 compounds are less than 2 ng·L−1, while 26 compounds range from 2 ng·L−1 to 10 ng·L−1, 19 compounds are at the range of 10–200 ng·L−1, and the other two compounds are 200 ng·L−1 and 1000 ng·L−1. Most of the recovery results were found to be between 60~130%. Finally, the method was successfully applied to the analysis of pesticide residues in 30 water samples from aquaculture environment in Shanghai, indicating its applicability in pesticide screening for environmental monitoring.
Highlights
The use of pesticides in agriculture plays an important role in preventing crop diseases, pests, rodents, etc., and promoting high quality and high yield of agricultural products [1].Due to the increases in demands of seafood, aquaculture has become one of the fastest growing food-production sectors [2]
Dionex Ultimate 3000 ultra-high-performance liquid chromatography coupled to a quadrupole/Orbitrap mass spectrometry (UHPLC-Q/Orbi MS) system operated in electrospray ionization (ESI) mode with Tracefinder analysis software (Q-Exactive, Thermo Fisher Scientific) was used to detect the pesticides
In order to evaluate the performance of the solid-phase extraction (SPE) enrichment, the blank aquaculture water samples spiked with all analytes at the concentration of 2 ng·L−1, 10 ng·L−1, 40 ng·L−1, and 200 ng·L−1 were enriched with SPE, eluted through mixed solvent, and were analyzed by the UHPLC-Q/Orbi MS system to examine the number of targets that can be identified and confirmed under different spiked amounts
Summary
The use of pesticides in agriculture plays an important role in preventing crop diseases, pests, rodents, etc., and promoting high quality and high yield of agricultural products [1]. The pesticide pollution in aquaculture water is of less concern, which is important for the quality and safety of aquatic products and water ecosystems. A fast, simple, and reliable method based on a one-step SPE enrichment-cleanup-elution strategy, followed by ultra-high-performance liquid chromatography (UHPLC) quadrupole/Orbitrap mass spectrometry (Q/Orbi MS) for screening of pesticides in water was established for the adequate monitoring of the pesticide residues in environment. A total of 80 target analytes, including organophosphorus, organochlorines, carbamates, imidazoles, triazines, phenylpyrazoles, avermectins, pyrethroids, and other pesticides, were successfully screened. These compounds were frequently used as insecticides and fungicides in water and negatively impact human health [3,33]. 30 environmental water samples from different regions of rivers, lakes, and aquaculture environment in Shanghai were screened with this method
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