Development and Independent Laboratory Validation of an Analytical Method for the Direct Determination of Glyphosate, Glufosinate, and Aminomethylphosphonic Acid in Honey by Liquid Chromatography/Tandem Mass Spectrometry
DOI:
https://doi.org/10.21423/JRS-V05N02P001Keywords:
glyphosate, honey, LC/MSAbstract
A simple high-throughput liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed for the determination of glyphosate, glufosinate and aminomethylphosphonic acid (AMPA) in honey using a reversed-phase column with weak anion-exchange and cation-exchange mixed-mode. One gram of sample was shaken with water containing ethylenediaminetetraacetic acid disodium salt and acetic acid for five minutes. After centrifugation, the supernatant was mixed with internal standard and directly injected and analyzed in ten minutes by LC-MS/MS with no sample concentration or derivatization steps. Two precursor/product ion transitions were monitored in the method for each target compound to achieve true positive identification. Three isotopically labelled internal standards corresponding to each analyte were used to correct for matrix suppression effects and/or instrument signal drift. The average recovery for all analytes at 25, 50, 100, and 500 ng/g (n=11) ranged from 87 to 111% with a relative standard deviation of less than 12%.
https://doi.org/10.21423/jrs-v05n02p001 (DOI assigned 3/11/2019)
References
Alferness, P. L., & Iwata, Y. (1994). Determination of glyphosate and (aminomehtyl) phosphonic acid in soil, plant and animal matrices, and water by capillary gas chromatography with mass selective detection. Journal of Agricultural and Food Chemistry, 42, 2751-2759.
Anastassiades, M., Kolberg, D. I., Eichhorn, E., Benkenstein, A., Lukacevic, S., Mack, D., Wildgrube, C., Sigalov, I., Dork, D., & Barth, A. (n.d.). Retrieved January 27, 2015, from http://www.crl-pesticides.eu/library/docs/srm/meth_QuPPe.pdf
Botero-Coy, A. M., Ibanez, M., Sancho, J. V., & Hernandez, F. (2013). Direct liquid chromatography–tandem mass spectrometry determination of underivatized glyphosate in rice, maize and soybean. Journal of Chromatography: A, 1313, 157-165.
Chamkasem, N., Harmon, T., & Morris, C. (2015). Food and Drug Administration, Office of Regulatory Affairs. Direct determination of glyphosate, glufosinate, and AMPA in milk by liquid chromatography/tandem mass spectrometer (Laboratory Information Bulletin No. 4595).
Chamkasem, N., Harmon, T., & Morris, C. (2015). Food and Drug Administration, Office of Regulatory Affairs. Direct determination of glyphosate, glufosinate, and AMPA in soybean and corn by liquid chromatography/tandem mass spectrometer (Laboratory Information Bulletin No. 4596).
Hao, C., Morse, D., Morra, F., Zhao, X., Yang, P., & Nunn, B. (2011). Direct aqueous determination of glyphosate and related compounds by liquid chromatography/tandem mass spectrometer using reversed-phase and weak anion-exchange mixed-mode column. Journal of Chromatography: A, 1218, 5638-5643.
Hogendoorn, E. A., Ossendrijver, F. M., Dijkman, E., & Baumann, R. A. (1999). Rapid determantiaon of glyphosate in cereal samples by means of pre-column derivatization with 9-fluorenylmethayl chloroformate and coupled-colun liquid chromatography with flourescence detection. Journal of Chromatography: A, 833, 1 67-73.
Honey: Nutritional and Sugar Profile. (n.d.). In Wikipedia. Retrieved January 5, 2016 from https://en.wikipedia.org/wiki/Honey#Nutritional_and_sugar_profile
Ibanez, M. P., Ozo, O. J., Sancho, J. V., Lopez, F. J., & Hernandez, F. (2005). Residue determination of glyphosate, glufosinate and aminomethylphosphonic acid in water and soil samples by liquid chromatography coupled to electrospray tandem mass spectrometry. Journal of Chromatography: A, 1081, 145-155.
Nagatomi, Y., Yoshioka, T., Yanagisawa, M., Uyama, A., & Mochizuki, N. (2013). Simultaneous LC-MS/MS analysis of glyphosate, glufosinate, and their metabolic products in beer, barley tea, and their ingredients. Bioscience, Biotechnology, and Biochemistry, 77, 2218-2221.
PAN Germany. (2017). Glyphosate: Severe Concerns Raised by New Facts [Press release]. Retrieved June 1, 2017 from http://www.pan-germany.org/deu/~news-1458.html
Qian, K., Tang, T., Shi, T., Li, P., & Cao, P. (2009). Solid-phase extraction and residue determination of glyphosate in apple by ion-pairing reverse-phase chromatography with pre-column derivatization. Journal of Separation Scence, 32, 2494-2300.
Robio, F., Guo, E., & Kamp, L. (2014). Survey of glyphosate residues in honey, corn and soy products. Journal of Environmental and Analytical Toxicology, 5:249.
Schreiber, A., & Cabrices, O. G. (2013). Automated Derivatization, SPE Cleanup and LC-MS/MS Determination of Glyphosate and Other Polar Pesticides. Retrieved January 1, 2015 from http://www.newfoodmagazine.com/wp-content/uploads/Glyphosate_QTRAP-4500_Gerstel_AB-SCIEX_8013813-01.pdf
U.S. Environmental Protection Agency. (n.d.). Pesticide Market Estimates. Retrieved January 1, 2015 from https://www.epa.gov/pesticides/pesticides-industry-sales-and-usage-2006-and-2007-market-estimates
Vreeken, R. J., Speksnijder, P., Bobeldijk-Pastorova, I. & Noij, Th. H. M. (1998). Selective analysis of the herbicides glyphosate and aminomethylphosphonic acid in water by on-line solid-phase extraction-high-performance liquid chromatography electrospray ionization mass spectrometry. Journal of Chromatography: A, 794, 187-199.
Downloads
Published
Issue
Section
License
This work is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.
By submitting content to the Journal of Regulatory Science (JRS), authors agree to the following terms:
- Authors retain copyright and grant the JRS the right of first publication. Authors retain patent, trademark, and other intellectual property rights (including research data) and grant third parties the right to use, reproduce, and share the article according to the Creative Commons — Attribution-NonCommercial 4.0 International — CC BY-NC 4.0 license agreement. The JRS is an open access journal and, as a result, articles are free to use with proper acknowledgment of the work's authorship and initial publication in this journal.
- Authors are permitted and encouraged to post their work online (e.g., in institutional repositories or on their website) prior to and during the submission process.
- If excerpts from other copyrighted works are included, the author(s) must obtain written permission from the copyright owners and credit the source(s) in the article.
- The publication of the submission has been approved by all co-authors and responsible authorities at the institute or organization where the work has been carried out.
- Copyright has not been breached in seeking publication of the submission.
