Novel Two-Stage Fine Milling Enables High-Throughput Determination of Glyphosate Residues in Raw Agricultural Commodities.

Dramatic process-efficiency gains for residue analysis of glyphosate in raw agricultural commodities (RACs) were achieved by development and validation of a two-stage fine-milling process. This secondary milling produced a uniform and consistent product that could be reproducibly measured with 75 mg analytical test portions. The milligram scale sample size enabled the direct weighing of sample into a liquid-handler-compatible 96-well format. A high-throughput workflow based on this innovative comminution approach for the quantitation of glyphosate, a nonselective herbicide, and its main degradation product, aminomethylphosphonic acid, was validated in various RACs and used to demonstrate the applicability of the two-step milling process. The precision and reproducibility of 75 mg analytical portions taken through this assay was used to demonstrate the feasibility of using a two-stage fine-milling technique for pesticide residue applications. An RSD of less than 10% was achieved in endogenous glyphosate residues in multiple RACs. Comparable recoveries and superior precision were achieved with this new method as compared with a validated 10 g scale method.