Pesticides in Seaweed: Optimization of Pressurized Liquid Extraction and in-Cell Clean-up and Analysis by Liquid Chromatography-Mass Spectrometry
Abstract
Chemical residues, such as insecticides and anthelmintics, are frequently redistributed from the aquatic environment to marine species. This work reports on a fast validated protocol for the analysis of azamethiphos, three avermectins, two carbamates and two benzoylurea pesticides and chemotherapeutic agents in seaweeds based on pressurized liquid extraction and separation of analytes by liquid chromatography coupled with tandem mass spectrometry. The variables affecting the efficiency of pressurized liquid extraction, including temperature, number of extraction cycles, static extraction time and percent acetonitrile flush volume, were studied using a Doehlert design. The optimum parameters were 100 °C and one cycle of 3 min with 70 % acetonitrile. Adequate in-cell clean-up of the seaweeds was achieved using 0.8 g of Florisil over 0.1 g of graphitized carbon black on the bottom of the cell. The optimized method was validated using an analyte-free seaweed sample fortified at different concentrations. The limits of quantification ranged from 3.6 μg kg(-1) (azamethiphos) to 31.5 μg kg(-1) (abamectin). The recovery was from 87 to 120 % in most cases at different spiking levels. Finally, the reproducibility of the method expressed as the relative standard deviation and evaluated at concentrations of 10 and 50 μg kg(-1) was in the range 9-14.3 % and 6.1-12.3 %, respectively. The applicability of the method was evaluated with five commercial and 12 wild edible seaweeds, and four target compounds were detected in two wild seaweeds at a concentration below the quantification limit.
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Azophos, lufenuron, teflubenzuron, and propoxur have been detected in algae food using HPLC-MS.
“In another study, Lorenzo R et al. (2012) used high-performance liquid chromatography-mass spectrometry (HPLC-MS) to analyze pesticide content and the type of pesticide residues, such as azophos, lufenuron, teflubenzuron, and propoxur, have been detected in algae food [109].”
From Current Status and Future Trends in Removal, Control, and Mitigation of Algae Food Safety Risks for Human Consumption (2022) · cites this paper as [109]
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Food Safety Hazards in the European Seaweed Chain
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- Authors
- Lorenzo, R. A., Pais, S., Racamonde, I., García-Rodríguez, D., & Carro, A. M.
- Affiliations
- Universidade de Santiago de Compostela (ES)
- Corresponding author
- Lorenzo, R. A.
- Carro, A. M.
- Venue
- Analytical and Bioanalytical Chemistry
- Published
- 2012-05-26
- Volume
- 404
- Issue
- 1
- Pages
- 173-181
- ISSN
- 1618-2642 (ISSN-L)
- 1618-2650
- OpenAlex
- W1997601807
- Cited by
- 18
- References
- 35
- Citations by year
- 2024: 2 · 2022: 1 · 2021: 2 · 2020: 2 · 2017: 1 · 2015: 2 · 2014: 5 · 2013: 3
- FWCI
- 4.91
- Type
- journal article
- Language
- en
- Open access
- closed
- Licence
- www.springer.com/tdm (tdm)
- Locations
- Analytical and Bioanalytical Chemistry (publishedVersion)
- PubMed (publishedVersion)
- Topics
- Life Sciences › Agricultural and Biological Sciences › Food Science › Pesticide Residue Analysis and Safety
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Environmental Science › Health, Toxicology and Mutagenesis › Environmental Toxicology and Ecotoxicology
- Keywords
- pesticide residues, seaweed, azamethiphos, avermectin, carbamates, benzoylurea, Doehlert design, Florisil, graphitized carbon black, edible seaweeds, marine pollution, insecticides, anthelmintics
- MeSH terms
- Chromatography, Liquid, Food Contamination, Pesticides, Seaweed, Tandem Mass Spectrometry, Liquid-Liquid Extraction
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