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Qualitative/quantitative strategy for the determination of glufosinate and metabolites in plants

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Abstract

A simple method for the simultaneous determination of glufosinate and its metabolites in plants based on liquid chromatography–ultraviolet (LC–UV) absorption detection after derivatization with fluorenylmethoxycarbonyl chloride (FMOC-Cl) of some analytes to facilitate separation is reported here. Nonavailable standard metabolites were identified by LC–TOF/mass spectrometry (MS), which also confirmed all target analytes. Ultrasound-assisted extraction was used for sample preparation (power of 70 W and duty cycle of 0.7 s/s for 10 min) with subsequent evaporation of the extractant, reconstitution and filtration as the cleanup/concentration step prior to derivatization, and chromatographic separation and detection at 270 nm for underivatized analytes and 340 nm for those that were derivatized. The chromatographic analysis was completed in 40 min using a Luna® column (C18 phase). The analytical characteristics of the method were linear dynamic range of the calibration curves within 0.047–700 μg/mL with a regression coefficient (rc) of 0.999 for glufosinate, 0.077–700 μg/mL with a rc of 0.998 for N-acetyl-glufosinate, and 0.116–600 μg/mL with a rc of 0.998 for 3-(methylphosphinico)propanoic acid. The precision for the determination of glufosinate (studied at two levels, 0.1 and 5 μg/mL) was 2.7 and 6.0 % for repeatability and 4.7 and 7.2 % for within-laboratory reproducibility, respectively. Identification and confirmatory analysis of the presence of glufosinate and metabolites in the extracts from treated plants was carried out by LC–TOF/MS in high-resolution mode for the precursor ion. The method was validated by analyzing wheat (Triticum aestivum) samples (resistant and susceptible biotypes) treated with 300 g of glufosinate/ha following conventional agronomical practices.

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Acknowledgments

The authors thank the Spanish Ministerio de Ciencia e Innovación (MICINN) and FEDER program for the financial support through Project Nos. AGL-2010 16774 and CTQ2012-37428. F.P.C. is also grateful to the MICINN for a Ramón y Cajal contract (RYC-2009-03921).

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The authors declare no conflict of interest.

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Authors and Affiliations

  1. Department of Agricultural Chemistry, University of Córdoba, C-3 Building, Campus of Rabanales, 14071, Córdoba, Spain

    A. M. Rojano-Delgado & R. De Prado

  2. Department of Analytical Chemistry, University of Córdoba, Annex C-3, Campus of Rabanales, 14071, Córdoba, Spain

    F. Priego-Capote & M. D. Luque de Castro

  3. University of Córdoba, Agroalimentary Excellence Campus, ceiA3, 14071, Córdoba, Spain

    A. M. Rojano-Delgado, F. Priego-Capote, R. De Prado & M. D. Luque de Castro

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  1. A. M. Rojano-Delgado
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  2. F. Priego-Capote
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  3. R. De Prado
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  4. M. D. Luque de Castro
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Correspondence to M. D. Luque de Castro.

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Rojano-Delgado, A.M., Priego-Capote, F., De Prado, R. et al. Qualitative/quantitative strategy for the determination of glufosinate and metabolites in plants. Anal Bioanal Chem 406, 611–620 (2014). https://doi.org/10.1007/s00216-013-7484-y

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  • DOI: https://doi.org/10.1007/s00216-013-7484-y

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