A simplified approach to the determination of N-nitroso glyphosate in technical glyphosate using HPLC with post-derivatization and colorimetric detection

Talanta. 2007 May 15;72(3):1054-8. doi: 10.1016/j.talanta.2006.12.047. Epub 2007 Jan 12.

Abstract

A simple and sensitive HPLC post-derivatization method with colorimetric detection has been developed for the determination of N-nitroso glyphosate in samples of technical glyphosate. Separation of the analyte was accomplished using an anionic exchange resin (2.50mmx4.00mm i.d., 15mum particle size, functional group: quaternary ammonium salt) with Na(2)SO(4) 0.0075M (pH 11.5) (flow rate: 1.0mLmin(-1)) as mobile phase. After separation, the eluate was derivatized with a colorimetric reagent containing sulfanilamide 0.3% (w/v), [N-(1-naphtil)ethilendiamine] 0.03% (w/v) and HCl 4.5M in a thermostatized bath at 95 degrees C. Detection was performed at 546nm. All stages of the analytical procedure were optimized taking into account the concept of analytical minimalism: less operation times and costs; lower sample, reagents and energy consumption and minimal waste. The limit of detection (k=3) calculated for 10 blank replicates was 0.04mgL(-1) (0.8mgkg(-1)) in the solid sample which is lower than the maximum tolerable accepted by the Food and Agriculture Organization of the United Nations.