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Ultratrace-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in natural waters by solid-phase extraction followed by liquid chromatography–tandem mass spectrometry: performance tuning of derivatization, enrichment and detection
Open accessAbstract
A sensitive and robust analytical method for the quantification of glyphosate, aminomethylphosphonic acid (AMPA) and glufosinate in natural water has been developed on the basis of a derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl), solid-phase extraction (SPE) and liquid chromatography followed by electrospray tandem mass spectrometry (LC-ESI-MS/MS). In order to maximize sensitivity, the derivatization was optimized regarding organic solvent content, amount of FMOC-Cl and reaction time. At an acetonitrile content of 10% a derivatization yield of 100% was reached within two hours in groundwater and surface water samples. After a twofold dilution the low acetonitrile content allowed solid-phase extraction of a sample of originally 80 mL over 200 mg Strata-X cartridges. In order to decrease the load of the LC column and mass spectrometer with derivatization by-products (e.g., 9-fluorenylmethanol FMOC-OH), a rinsing step was performed for the SPE cartridge with dichloromethane. Acidification of the sample and addition of EDTA was used to minimize complexation of the target compounds with metal ions in environmental samples. Due to the large sample volume and the complete FMOC-OH removal, limits of quantification of 0.7 ng/L, 0.8 ng/L and 2.3 ng/L were achieved in surface water for glyphosate, AMPA and glufosinate, respectively. The limits of detection were as low as 0.2 ng/L, 0.2 ng/L and 0.6 ng/L for glyphosate, AMPA and glufosinate, respectively. Surface water and ground water samples spiked at 2 ng/L showed recoveries of 91-107%.
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Amines are also found in anthracyclines, such as doxorubicin, and aminoglycosides such as gentamicin.
“They are also found in anthracyclines, such as the antineoplastic drug doxorubicin, and aminoglycosides such as the antibiotic gentamicin.112,114,115”
From Connecting metabolome and phenotype: recent advances in functional metabolomics tools for the identification of bioactive natural products (2024) · cites this paper as [115]
The Introduction and Chemicals sections discuss glyphosate, AMPA, and glufosinate, while the Concentration of FMOC Cl section mentions other amines generally. Searches for doxorubicin, gentamicin, anthracyclines, aminoglycosides, and amines in drugs found no passage addressing the claimed examples; page numbers were unavailable. (LLM, conf=0.76)
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Derivatization for liquid chromatography-mass spectrometry
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Metadata
- Authors
- Hanke, I., Singer, H., & Hollender, J.
- Affiliations
- Swiss Federal Institute of Aquatic Science and Technology (CH)
- Corresponding author
- Singer, Heinz
- Venue
- Analytical and Bioanalytical Chemistry
- Published
- 2008-05-16
- Volume
- 391
- Issue
- 6
- Pages
- 2265-2276
- ISSN
- 1618-2642 (ISSN-L)
- 1618-2650
- OpenAlex
- W2058038407
- Cited by
- 194
- References
- 25
- Citations by year
- 2026: 5 · 2025: 9 · 2024: 6 · 2023: 16 · 2022: 11 · 2021: 16 · 2020: 16 · 2019: 17 · 2018: 15 · 2017: 7 · 2016: 11 · 2015: 13 · 2014: 8 · 2013: 8 · 2012: 10
- FWCI
- 13.86
- Type
- journal article
- Language
- en
- Open access
- green
- www.dora.lib4ri.ch
- Licence
- other-oa
- www.springer.com/tdm (tdm)
- Locations
- Analytical and Bioanalytical Chemistry (publishedVersion)
- PubMed (publishedVersion)
- reroDoc Digital Library (submittedVersion)
- DORA Eawag (Swiss Federal Institute of Aquatic Science and Technology (Eawag)) (submittedVersion, other-oa)
- RWTH Publications (RWTH Aachen) (submittedVersion)
- Funders
- Bundesamt für Umwelt
- Topics
- Life Sciences › Agricultural and Biological Sciences › Food Science › Pesticide Residue Analysis and Safety
- Physical Sciences › Environmental Science › Pollution › Pesticide and Herbicide Environmental Studies
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Keywords
- glyphosate, aminomethylphosphonic acid, glufosinate, herbicide residues, natural waters, groundwater, surface water, solid-phase extraction, metal complexation, ultra-trace detection
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