Microextraction technique associated with gas chromatography–mass spectrometry for determining pesticide residues in urine.
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| Title: | Microextraction technique associated with gas chromatography–mass spectrometry for determining pesticide residues in urine. |
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| Authors: | Silva, Thaís L. R.1 (AUTHOR), de Queiroz, Maria Eliana L. R.1 (AUTHOR), de Oliveira, André Fernando1 (AUTHOR), Rodrigues, Alessandra A. Z.1,2 (AUTHOR), Neves, Antônio Augusto1 (AUTHOR), Vieira, Patrícia A. F.3 (AUTHOR), de Queiroz, José Humberto4 (AUTHOR), Barbosa, Verônica O. de P.1 (AUTHOR) |
| Source: | Journal of Environmental Science & Health. Part B. Pesticides, Food Contaminants & Agricultural Wastes. 2022, Vol. 57 Issue 3, p165-175. 11p. |
| Subject Terms: | *Pesticide residues in food, *Pesticides, *Pesticide pollution, *Gas chromatography/Mass spectrometry (GC-MS), *Mass spectrometry, Urine, Liquid-liquid extraction, Factorial experiment designs |
| Abstract: | Urine is one of the biological matrices most used for detecting human contamination, as it is representative and easily obtained via noninvasive sampling. This study proposes a fast, accurate, and ecological method based on liquid–liquid microextraction with low-temperature partition (μLLE/LTP). It was validated to determine nine pesticides (lindane, alachlor, aldrin, chlorpyrifos, dieldrin, endrin, DDT, bifenthrin, and permethrin) in human urine, in association with gas chromatography coupled with mass spectrometry (GC–MS). The technique was optimized through a factorial design. The best conditions for the simultaneous extraction of the analytes comprised the addition of 600 µL of water and 600 µL of acetonitrile (extracting solvent) to a 500-µL urine sample, followed by vortexing for 60 s. By freezing the samples for 4 h, it was possible to extract the pesticides and perform the extract clean-up simultaneously. The parameters selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy were used to appraise the performance of the method. Good values of selectivity and linearity (R2 > 0.990), LOQ (0.39–1.02 μg L−1), accuracy (88–119% recovery), and precision (%CV ≤ 15%) were obtained. The μLLE/LTP–GC–MS method was applied to authentic urine samples collected from volunteers in Southeast Brazil. [ABSTRACT FROM AUTHOR] |
| Copyright of Journal of Environmental Science & Health. Part B. Pesticides, Food Contaminants & Agricultural Wastes is the property of Taylor & Francis Ltd and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) | |
| Database: | GreenFILE |
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| Abstract: | Urine is one of the biological matrices most used for detecting human contamination, as it is representative and easily obtained via noninvasive sampling. This study proposes a fast, accurate, and ecological method based on liquid–liquid microextraction with low-temperature partition (μLLE/LTP). It was validated to determine nine pesticides (lindane, alachlor, aldrin, chlorpyrifos, dieldrin, endrin, DDT, bifenthrin, and permethrin) in human urine, in association with gas chromatography coupled with mass spectrometry (GC–MS). The technique was optimized through a factorial design. The best conditions for the simultaneous extraction of the analytes comprised the addition of 600 µL of water and 600 µL of acetonitrile (extracting solvent) to a 500-µL urine sample, followed by vortexing for 60 s. By freezing the samples for 4 h, it was possible to extract the pesticides and perform the extract clean-up simultaneously. The parameters selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy were used to appraise the performance of the method. Good values of selectivity and linearity (R2 > 0.990), LOQ (0.39–1.02 μg L−1), accuracy (88–119% recovery), and precision (%CV ≤ 15%) were obtained. The μLLE/LTP–GC–MS method was applied to authentic urine samples collected from volunteers in Southeast Brazil. [ABSTRACT FROM AUTHOR] |
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| ISSN: | 03601234 |
| DOI: | 10.1080/03601234.2022.2038505 |
