Analysis of Glyphosate and Aminomethylphosphonic Acid in Nutritional Ingredients and Milk by Derivatization with Fluorenylmethyloxycarbonyl Chloride and Liquid Chromatography Mass Spectrometry

A straightforward analytical method based on derivatization with fluorenylmethyloxycarbonyl chloride and liquid chromatography mass spectrometry has been developed for the analysis of residues of glyphosate and aminomethylphosphonic acid (AMPA) in a suite of nutritional ingredients derived from soybean, corn, and sugar beet and also in cow's milk and human breast milk. Accuracy and intermediate precision were 91-116% and <10% RSD, respectively, in soy protein isolate. Limits of quantitation were 0.05 and 0.005 mu g/g in powdered and liquid samples, respectively. Glyphosate and AMPA were quantified at 0.105 and 0.210 mu g/g (soy protein isolate) and 0.850 and 2.71 mu g/g (soy protein concentrate, both derived from genetically modified soybean), respectively. Residues were not detected in soy milk, soybean oil, corn oil, maltodextrin, sucrose, cow's milk, whole milk powder, or human breast milk. The method is proposed as a convenient tool for the survey of glyphosate and AMPA in the ingredient supply chain.