Methods were developed to determine glufosinate (GLUF), glyphosate (GLYP) and its metabolite, aminomethylphosphonic acid (AMPA) by capillary electrophoresis-laser induced fluorescence detection using 5-(4,6-dichlorotriazinylamino) fluorescein (DTAF) and fluorescein isothiocyanate (FITC) as the derivatizing reagents. To accelerate the labeling speed, a microwave-assisted derivatization method was adopted. The derivatizing reaction time was reduced to 180 and 150 s for DTAF and FITC, whose reaction time for conventional labeling was 50 min and 5 h, respectively. The optimum separation conditions for derivatives were as follows: a back ground electrolyte (BGE) of 30 mmol L -1 sodium tetraborate containing 15 mmol L -1 brij-35, hydrodynamic injection 15 s and a 10 kV separation voltage. Under these conditions, the LODs (S/N = 3) for DTAF derivatives were 0.32, 0.19 and 0.15 nmol L -1 for GLUF, GLYP, and AMPA, respectively. The LODs (S/N = 3) for FITC derivatives were 2.60, 3.88 and 2.42 nmol L -1 for GLUF, GLYP, and AMPA, respectively. The applicability of the developed method was demonstrated by the detection of the above herbicides and metabolite in water and soil samples.
A sensitive analytical method was developed for the simultaneous determination of glyphosate, glufosinate and aminomethylphosphonic acid by capillary electrophoresis with laser-induced fluorescence detection (CE-LIF). 5-(4,6-Dichlorotriazinyl) amino fluorescein (DTAF) was successfully applied to label the herbicides. The optimal derivatization reaction was carried out in boric acid buffer of pH 9.5 at 30 degrees C for 40 min. The baseline separation of the three derivatives could be accomplished using 30 mmol/L boric acid, 15 mmol/L Brij-35 (pH 9.5) as the running buffer. The detection limits (S/N = 3) for the glyphosate, glufosinate and aminomethylphosphonic acid were 3.21, 6.14, 1.99 ng/kg, respectively. Finally, the method was successfully applied to the analysis of environmental samples, and the three compounds were measured without any interference from real samples. The recoveries of the compounds in these samples were 91.3% - 106.0%. The method has the advantages of easiness and sensitivity, and can meet the requirement of the determination of the herbicide and metabolite residues in the environmental samples.
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