Study of the Reaction Derivatization Glyphosate and Aminomethylphosphonic Acid (AMPA) with <i>N</i>,O-Bis(trimethylsilyl)trifluoroacetamide

Abstract

This work aimed to study the derivatization unprecedented of glyphosate and AMPA solutions using N,O-bis (trimethylsilyl)trifluoroacetamide (BSTFA) combined with trimethylchlorosilane (TMCS), evaluating the composition of the reaction medium, use of ultrasound, volume of BSTFA:pyridine and pH of the reaction medium. From this study it was inferred that the reaction medium was composed of BSTFA:pyridine in ratio 60:100, respectively, without ultrasonic vibration and pH adjustment that provide optimal conditions for analysis by GC-MS. Furthermore, the methodology used was simple and fast, and that was the most practical method commonly used.

The role of derivatization techniques in the analysis of glyphosate and aminomethyl-phosphonic acid by chromatography

“…As to the analytical performance characteristics, in spite of selective acquisition processes (GC-MS and GC-MS-SIM), because of methods' low sensitivity they have not been full documented [18,28,35,41,42,46,47]; few have been presented with numerical data. Reliable values, suitable for serum and urine analyses [28,35,46] were found, only.…”

“…Reliable values, suitable for serum and urine analyses [28,35,46] were found, only. In three papers [18,41,47] neither LOD nor LOQ data were given.…”

“…Forced techniques (90°C, 150 min) with 10% TMCS catalyst, proved to be less comfortable [41] than the use of a beneficial reagent medium (BSTFA:PYR, in ratio 0.6:1, v/v) resulting in a fast, practically utilizable method [47].…”

“…This popular technique was optimized partly for basic research studies [18,41,47], partly to determine herbicide poisoning via serum and urine analysis [28,35,42,46]. MTBSTFA was declared as the right reagent selection, providing the expected molecular ions of three TBDMS groups (GLYP, [M] m/z, 511; AMPA m/z, [M] 451), and their characteristic fragment ions formed by the loss of common characteristic masses as a methyl (m/z 15) or a TBDMS (m/z 57) group, for both herbicides in question.…”

Extraction and Simultaneous Determination of Glyphosate, AMPA and Compounds of the Shikimic Acid Pathway in Plants

“…Several methods for determination of some of these compounds are reported both by spectrophotometry (Zelaya et al, 2011) and by liquid chromatography coupled to mass spectrometry (Raji et al, 2014) and detection by fluorescence (Zhang et al, 2013), or arrangement of photodiodes (Matallo et al, 2009;Alcaide-Molina et al, 2013) and gas chromatography with mass detector (Catrinck et al, 2013). However, the adoption of only one method of extraction and quantification of glyphosate, AMPA (aminomethylphosphonic acid) and compounds related to the shikimic acid pathway has not been reported.…”