Abstract

The official method for analyzing N-nitrosoglyphosate (NNG), a relevant impurity, in glyphosate matrix demands complicated instrumentation and operating conditions not available in many laboratories. In this work, we developed a direct, simple, selective and sensitive ion chromatography (IC) method with UV detection for the determination of NNG in samples of technical glyphosate. To separate NNG from the matrix we used an IC anionic column mounted in a high-performance liquid chromatography (HPLC) apparatus equipped with a photo-diode array detector. The system used a high ionic strength eluent. The method was validated, taking into account the following figures of merit: selectivity, linearity, repeatability, intermediate precision, recovery, limit of detection (LOD), and limit of quantification (LOQ). The proposed method is sensitive enough to quantify NNG below the maximum concentration determined by both the Food and Agricultural Organization of the United Nations (FAO) and the Brazilian regulation.

Highlights

  • The agriculture in Brazil is very dependent on the use of pesticides, and the country is one of the greatest pesticide consumers in the world.[1]

  • We moved the ion chromatography (IC) anion column from the ion chromatographic system and mounted it on the high-performance liquid chromatography (HPLC) system coupled with a diode array detector (DAD)

  • The development of a simple and direct method, sensitive enough to quantify this impurity at levels below legislated limits, can facilitate NNG control in technical pesticide products by reducing the costs and time of analysis

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Summary

Introduction

The agriculture in Brazil is very dependent on the use of pesticides, and the country is one of the greatest pesticide consumers in the world.[1] Glyphosate (GLY) or [N-(phosphonomethyl)glycine], the active ingredient (AI) most often used in Brazil, is classified as a non-selective, systemic and post-emergent herbicide. It is highly effective in weed control, but its carcinogenicity in humans is in the spotlight since IARC (International Agency for Research on Cancer) panel classified glyphosate in Category 2A (probably carcinogenic to humans).[2,3,4,5]. The samples were suspected of containing NNG in concentrations higher than the maximum level determined by INC 2/2008.10

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