Advanced Liquid Chromatography with Tandem Mass Spectrometry Method for Quantifying Glyphosate, Glufosinate, and Aminomethylphosphonic Acid Using Pre-Column Derivatization

Martin, P.; He, Ke; Blaney, Lee; Hobbs, Shakira R.

doi:10.1021/acsestwater.3c00094

Cited by 11 publications

(13 citation statements)

References 34 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Pre-column FMOC-Cl derivatization has been proven to be simple and successful. The complete reaction of glyphosate with FMOC-Cl guarantees stability and successful chromatographic separation on reversed-phase LC columns [ 33 ]. The derivatization takes place at an alkaline pH: generally, the pH is adjusted to 9 by adding borate buffer and by adding EDTA.…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

“…The derivatization takes place at an alkaline pH: generally, the pH is adjusted to 9 by adding borate buffer and by adding EDTA. With LC-MS/MS, the parent ions to be monitored are 390 m/z for glyphosate-FMOC and 332 m/z for AMPA-FMOC [ 33 , 34 ]. The daughter ions are frequently 150 m/z for glyphosate-FMOC and 110 m/z for AMPA-FMOC, so the transitions of interest are generally 390 → 150 m/z and 332 → 110 m/z [ 34 , 38 ], but also 168 → 63 m/z and 110 → 63 m/z in those cases where derivatization is not used [ 62 ].…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

“…The daughter ions are frequently 150 m/z for glyphosate-FMOC and 110 m/z for AMPA-FMOC, so the transitions of interest are generally 390 → 150 m/z and 332 → 110 m/z [ 34 , 38 ], but also 168 → 63 m/z and 110 → 63 m/z in those cases where derivatization is not used [ 62 ]. Detection can be carried out in positive electrospray mode [ 36 ] or in negative electrospray ionization mode [ 33 , 34 , 38 , 62 ]. The eluting solvents are often ammonium acetate in LC−MS-grade water, and acetonitrile (ACN).…”

Section: Chemical Analytical Methodsmentioning

confidence: 99%

“…The highly topical debate on a herbicide declared in the past to be of little danger currently requires more careful evaluations and a greater number of analytical measurements to understand its fate once used in the field and how much of it passes into the various final products intended for consumption, with the consequent degree of exposure for consumers. Due to some of its molecular characteristics (the absence of UV absorbance, low volatility, and high hydrophilicity) [ 1 , 30 , 31 , 32 , 33 ], the quantitative determination of glyphosate in crops, in soils, and in waters is challenging. Chromatography is the most successful and the most used technique, which, very frequently, exploits derivatization (mandatory in gas chromatography).…”

Section: Introductionmentioning

confidence: 99%

“…When liquid chromatography with derivatization is applied, the prevalent derivatizing agent is FMOC-Cl (9-fluorenylmethyl chloroformate). FMOC-Cl reacts with glyphosate and AMPA to give the corresponding derivatives [ 33 , 34 , 35 , 36 , 37 , 38 , 39 , 40 , 41 , 42 ]. The determination of glyphosate by liquid chromatography is also possible without derivatization.…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

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

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 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.

show abstract

Section: Chemical Analytical Methodsmentioning

confidence: 99%