Analysis of Glyphosate and Aminomethylphosphonic Acid in Nutritional Ingredients and Milk by Derivatization with Fluorenylmethyloxycarbonyl Chloride and Liquid Chromatography–Mass Spectrometry

Ehling, Stefan; Reddy, Todime M.

doi:10.1021/acs.jafc.5b04453

Cited by 55 publications

(42 citation statements)

References 25 publications

(67 reference statements)

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“…Stock solutions containing either one or the two analytes at 200 mg/L in 0.1 M HCl were prepared. Acidification with HCl to pH 1 has been found to be necessary in the case of environmental samples since multivalent cations form stable complexes with GLP and AMPA, which are not derivatized [11,20,[25][26][27]32,33]. All standard and working solutions were stored at 4 • C in polypropylene material given that GLP binds to active sites on glass when it is not derivatized [22,24,27].…”

Section: Reagents and Solutionsmentioning

confidence: 99%

“…However, other studies found optimum reaction times of 30 min [18,22,23] and 60 min [24]. Once the prefixed derivatization time is achieved, the solution must be acidified to stop the reaction and to obtain stable derivatives for some days [20][21][22][25][26][27]. Due to the stability of FMOC derivatives, this reagent is applied as a precolumn derivatization reaction.…”

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confidence: 99%

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Evaluation and optimization of the derivatization reaction conditions of glyphosate and aminomethylphosphonic acid with 6‐aminoquinolyl‐N‐hydroxysuccinimidyl carbamate using reversed‐phase liquid chromatography

Fontàs

Sánchez

2020

J of Separation Science

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Due to the polar and ionic characteristics of glyphosate and its main metabolite, aminomethylphosphonic acid, a derivatization reaction is required before performing liquid chromatographic determination of these compounds. In this study, reaction conditions using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate as the derivatization reagent are assessed. A two-level full-factorial design is applied here to optimize the derivatization time (ranging from 0.5 to 20 min) and temperature (from 24 to 55 • C). It is found that neither of these two variables have a significant effect on the derivatization process and that the reaction is quantitatively achieved in a few seconds at room temperature (24 • C). The results obtained indicate that derivatization reaction with 6-aminoquinolyl-Nhydroxysuccinimidyl carbamate is achieved in milder conditions, with a faster kinetic reaction, than those required with the most conventional derivatization reagents used today, and the derivatives are more stable. It has been found that the most important parameter affecting the chromatographic separation is the pH of the mobile phase, as it has a significant effect on the retention time of the hydrolyzed excess of reagent. When ammonium acetate is used in the mobile phase, buffered solutions at pH around 5.0 are required. K E Y W O R D S 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, aminomethylphosphonic acid, derivatization, glyphosate, reversed-phase liquid chromatography 1 INTRODUCTION Glyphosate (N-phosphonomethyl-glycine; GLP) is a broadspectrum systemic herbicide widely used as a crop desic-Article Related Abbreviations: AMPA, aminomethylphosphonic acid; AMQ, 6-aminoquinoline; AQC, 6-aminoquinolyl-N-hydroxysuccinimidyl Carbamate; FMOC, 9-fluorenylmethylchloroformate; GLP, glyphosate; OPA, o-phatalaldehyde; TFA, trifluoroacetic acid cant. It is one of the most commonly used herbicides in agriculture due to the development of glyphosate-resistant genetically modified crop varieties [1,2] and it is also widely applied for urban and residential weed control [3]. The global glyphosate market is projected to reach USD 12.54 billion by 2024, with a compound annual growth rate of 6.8% over the forecast period, from 2019 to 2024 [4]. GLP is considered to be nonpersistent in the environment as it degrades by microbial organisms in

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Section: Reagents and Solutionsmentioning

confidence: 99%

mentioning

confidence: 99%

Evaluation and optimization of the derivatization reaction conditions of glyphosate and aminomethylphosphonic acid with 6‐aminoquinolyl‐N‐hydroxysuccinimidyl carbamate using reversed‐phase liquid chromatography

Fontàs

Sánchez

2020

J of Separation Science

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“…Two papers published in 2015 reported the GLYP, AMPA, and GLUF determination in milk and milk-based products. Ehling and Reddy carried out a derivatization with FMOC-Cl followed by means of LC-MS/MS in different nutritional milk matrices such as cow's milk, human breast milk, soy milk, and whole milk powder [98]. This study is important because the reported analytical method does not require any analytical treatment such as clean-up, evaporation, or concentration; so, the possible artifact formation is drastically reduced.…”

Section: Beveragesmentioning

confidence: 99%

A Review of the Analytical Methods Based on Chromatography for Analyzing Glyphosate in Foods

Avino¹,

Notardonato²,

Russo³

2020

Pests, Weeds and Diseases in Agricultural Crop and Animal Husbandry Production

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Glyphosate is a pesticide widely used in agriculture, horticulture, and silviculture as well as around homes and gardens. It was introduced by Monsanto in the early 1970s, and it is a broad spectrum, nonselective, post-emergence herbicide that inhibits plants' shikimic acid pathway. Glyphosate is considered as "difficult herbicide" in terms of trace analysis. It has low molecular weight, low volatility, thermal lability, and good water solubility. These properties cause problems in its extraction, purification, and detection. The determination often requires additional processes that may allow quantification by chromatographic methods. Several analytical procedures have been developed based on solid-phase extraction, ion-exchange chromatography, or matrix solid phase dispersion. Most published methods involve liquid extraction followed by clean-up. This review would like to revise the literature on this issue discussing the relevant chromatographic methods reported in the literature in terms of analytical parameters for analyzing such compound in food chain.

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“…Overall, these methods are relatively complicated and time-consuming. Furthermore, the use of derivatization agent typically requires the nonvolatile buffer of borates to adjust the pH values, and the borates can result in signal instability and formation of salt deposits [19,20,31,32]. Besides avoiding the derivatizaiton step, this method also needs no preconcentration step for obtaining high sensitivity.…”

Section: Comparison To Previous Reportsmentioning

confidence: 99%

Sensitive, rapid and non-derivatized determination of glyphosate, glufosinate, bialaphos and metabolites in surface water by LC–MS/MS

Guo

Gao²,

Guo

et al. 2019

SN Appl. Sci.

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Glyphosate, glufosinate and bialaphos are widely used worldwide as herbicides. It has been reported that they can transfer into environmental water bodies, posing health threat to human. Thus, a sensitive and rapid analysis methodology for these compounds and corresponding metabolites is highly necessary. Due to their zwitterionic nature, previously reported methods for determination of these compounds generally require derivatization. Also, preconcentration step is typically needed in order to obtain high sensitivity. Herein, we report a very convenient and sensitive assay for these herbicides as well as corresponding metabolites in surface water. With judicious tuning of chromatographic conditions, very low LODs were achieved without derivatization or preconcentration step. The LODs were 0.15 ng mL −1 for glyphosate, glufosinate, MPPA and bialaphos, 0.1 ng mL −1 for AMPA. The LOQs were 0.5 ng mL −1 for glyphosate, glufosinate, MPPA and bialaphos, 0.3 ng mL −1 for AMPA. Recoveries ranging in 90.3-102.8% were obtained. The intra-day relative standard deviations (RSDs) ranged in 4.0-5.6%, while the inter-day RSDs ranged in 4.7-6.7%. The ME (n = 6) ranged from 92.6 to 97.2%. This assay was applied to real samples of surface water. This method is very promising for application in determination and routine monitoring of these compounds in environmental water bodies.

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Analysis of Glyphosate and Aminomethylphosphonic Acid in Nutritional Ingredients and Milk by Derivatization with Fluorenylmethyloxycarbonyl Chloride and Liquid Chromatography–Mass Spectrometry

Cited by 55 publications

References 25 publications

Evaluation and optimization of the derivatization reaction conditions of glyphosate and aminomethylphosphonic acid with 6‐aminoquinolyl‐N‐hydroxysuccinimidyl carbamate using reversed‐phase liquid chromatography

Evaluation and optimization of the derivatization reaction conditions of glyphosate and aminomethylphosphonic acid with 6‐aminoquinolyl‐N‐hydroxysuccinimidyl carbamate using reversed‐phase liquid chromatography

A Review of the Analytical Methods Based on Chromatography for Analyzing Glyphosate in Foods

Sensitive, rapid and non-derivatized determination of glyphosate, glufosinate, bialaphos and metabolites in surface water by LC–MS/MS

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