Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution

Junqué, Eva; Fernández, Pilar; Filippi, Iohanna; Grimalt, Joan O.

doi:10.1016/j.jcoa.2023.100087

Cited by 7 publications

(8 citation statements)

References 48 publications

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“…Other ions of interest are those derived from the loss of a CF 3 group (69 m/z ), which, for the HFB derivative of AMPA (571 amu), results in a 502 m/z ion fragment, while for the TFE derivative of AMPA (371 amu), it yields a 302 m/z ion fragment [ 124 ]. Other relevant ions in SIM mode or transitions that are exploited in tandem mass spectrometry are available from the literature [ 43 , 44 , 45 , 46 , 47 , 48 , 49 , 50 , 51 , 52 ]. Figure 8 shows the mass spectra of glyphosate and AMPA when derivatized with heptafluorobutanol and trifluoroacetic anhydride, as obtained in the work of Alferness and Iwata [ 123 ].…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

“…Methods Protoc. 2024, 7, x FOR PEER REVIEW 14 of 23 relevant ions in SIM mode or transitions that are exploited in tandem mass spectrometry are available from the literature [43][44][45][46][47][48][49][50][51][52]. Figure 8 shows the mass spectra of glyphosate and AMPA when derivatized with heptafluorobutanol and trifluoroacetic anhydride, as obtained in the work of Alferness and Iwata [123].…”

Section: Instrumental Setupmentioning

confidence: 99%

“…The determination of glyphosate by liquid chromatography is also possible without derivatization. As regards gas chromatography (GC), a largely used derivatization is that of using perfluoroalcohols plus trifluoroacetic anhydride [ 43 , 44 , 45 , 46 , 47 , 48 , 49 , 50 , 51 , 52 ]. The perfluoroalcohol used is trifluoroethanol (TFE) or heptafluorobutanol (HFB).…”

Section: Introductionmentioning

confidence: 99%

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Chromatographic Methods for the Determination of Glyphosate in Cereals Together with a Discussion of Its Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

Masci,

Caproni,

Nevigato

2024

MPs

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The European Union’s recent decision to renew the authorization for the use of glyphosate until 15 December 2033 has stimulated scientific discussion all around the world regarding its toxicity or otherwise for humans. Glyphosate is a chemical of which millions of tons have been used in the last 50 years worldwide to dry out weeds in cultivated fields and greenhouses and on roadsides. Concern has been raised in many areas about its possible presence in the food chain and its consequent adverse effects on health. Both aspects that argue in favor of toxicity and those that instead may indicate limited toxicity of glyphosate are discussed here. The widespread debate that has been generated requires further investigations and field measurements to understand glyphosate’s fate once dispersed in the environment and its concentration in the food chain. Hence, there is a need for validated analytical methods that are available to analysts in the field. In the present review, methods for the analytical determination of glyphosate and its main metabolite, AMPA, are discussed, with a specific focus on chromatographic techniques applied to cereal products. The experimental procedures are explained in detail, including the cleanup, derivatization, and instrumental conditions, to give the laboratories involved enough information to proceed with the implementation of this line of analysis. The prevalent chromatographic methods used are LC-MS/MS, GC-MS/SIM, and GC-MS/MS, but sufficient indications are also given to those laboratories that wish to use the better performing high-resolution MS or the simpler HPLC-FLD, HPLC-UV, GC-NPD, and GC-FPD techniques for screening purposes. The concentrations of glyphosate from the literature measured in wheat, corn, barley, rye, oats, soybean, and cereal-based foods are reported, together with its regulatory status in various parts of the world and its accumulation mechanism. As for its accumulation in cereals, the available data show that glyphosate tends to accumulate more in wholemeal flours than in refined ones, that its concentration in the product strictly depends on the treatment period (the closer it is to the time of harvesting, the higher the concentration), and that in cold climates, the herbicide tends to persist in the soil for a long time.

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Section: Chemical Analytical Methodsmentioning

confidence: 99%

Section: Instrumental Setupmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Chromatographic Methods for the Determination of Glyphosate in Cereals Together with a Discussion of Its Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

Masci,

Caproni,

Nevigato

2024

MPs

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“…Phosphorous (P) atom detection provides enhanced specificity and sensitivity with LOD 8.2 µg L -1 compared to LOD of HPLC 300 µg L -1 . Alone GC also helps in detection of GLY in different samples but when it is coupled with tandem mass spectrometry and isotope labelled standards it provides more selectivity and sensitivity with low LOD (0.05 µg L -1 ), overcoming any possible matrix effects 47 .…”

Section: Please Do Not Adjust Marginsmentioning

confidence: 99%

Glyphosate: a review on its widespread prevalence and occurrence across various systems

Ahuja,

Kumar,

Kumar

et al. 2024

Environ. Sci.: Adv.

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“…Other Other ions of interest are those derived from the loss of a CF 3 group (69 m/z), which, for the HFB derivative of AMPA (571 amu), results in a 502 m/z ion fragment, while for the TFE derivative of AMPA (371 amu), it yields a 302 m/z ion fragment [124]. Other relevant ions in SIM mode or transitions that are exploited in tandem mass spectrometry are available from the literature [43][44][45][46][47][48][49][50][51][52]. Figure 8 shows the mass spectra of glyphosate and AMPA when derivatized with heptafluorobutanol and trifluoroacetic anhydride, as obtained in the work of Alferness and Iwata [123].…”

Section: Instrumental Setupmentioning

confidence: 99%

Glyphosate as Contaminant in Cereals: Chromatographic Methods for Its Determination. Discussion about Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

Masci,

Caproni,

Nevigato

2024

Preprint

View full text Add to dashboard Cite

The European Union's recent decision to renew the authorization for the use of glyphosate until 15 December 2033 stimulates the scientific discussion all around the world regarding its toxicity or otherwise for humans. Glyphosate is a chemical used by millions of tons in the last 50 years worldwide to drying weeds in cultivated fields, greenhouses, roadsides. Concern has been raised in many quarters about the possible presence in the food chain and the consequent adverse effects on health: both aspects that argue in favor of toxicity and those that instead may indicate limited toxicity of glyphosate are here discussed. The great debate that has been generated requires further investigations and field measurements to understand its fate once dispersed in the environment and its concentration in the food chain. Hence the need for validated analytical methods that are available to analysts in the field. In the present review, methods for the analytical determination of glyphosate and its main metabolite, AMPA, are discussed, with a specific focus on chromatographic techniques applied to cereal products. The experimental procedures are explained in any detail, including cleanup, derivatization, and instrumental conditions to give the laboratories involved enough information to proceed with the implementation of this line of analysis. The prevalent chromatographic methods used are LC-MS/MS, GC-MS/SIM, and GC-MS/MS but sufficient indications are also given to those laboratories that wish to use the simpler HPLC-FLD, HPLC-UV, GC-NPD or GC-FPD techniques for screening purposes. Concentrations from literature measured in wheat, corn, barley, rye, oats, soybean, and cereal-based foods are reported together with the regulatory status in various parts of the world and the accumulation mechanism. As for the accumulation in cereals, available data show that glyphosate tends to accumulate more in wholemeal flours than in refined ones, that its concentration in the product strictly depends on the treatment period (the closer it is to the time of harvesting, the higher the concentration) and that in cold climates the herbicide tends to persist in the soil for a long time.

show abstract

Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution

Cited by 7 publications

References 48 publications

Chromatographic Methods for the Determination of Glyphosate in Cereals Together with a Discussion of Its Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

Chromatographic Methods for the Determination of Glyphosate in Cereals Together with a Discussion of Its Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

Glyphosate: a review on its widespread prevalence and occurrence across various systems

Glyphosate as Contaminant in Cereals: Chromatographic Methods for Its Determination. Discussion about Occurrence, Accumulation, Fate, Degradation, and Regulatory Status

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