Optimized Derivatization Procedure for Characterizing (Aminomethyl)phosphonic Acid Impurities by GC-MS

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

“…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.…”

“…BSTFA derivatization was suggested to the impurity profiling of AMPA and GLYP, only [41,47]. 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].…”

“…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.…”

“…Probably, this reagent pair might offer exponentially high responses). Table 3 Analysis of glyphopsate and AMPA by gas chromatograpy (GC), derivatized with N-Methyl-N-tert-butyldimethylsilyltrifluoroacetamide (MTBSTFA [18,28,35,42,46]) and with bistrimethylsilyl trifluoroacetamide (BSTFA [41,47] [47] Indications, as in Tables 1A, 1B Indications, as in Tables 1A, B, 2 As to the analytical performance characteristics, it is worth underlining the comparable efficiency of mass spectrometric and fluorescence detections. Certainly, it is a matter of compromise taking into consideration the type and amount of sample matrix, the derivatization reagent and effect of interactive parameters involved in the process.…”