Abstract
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 μg/g in powdered and liquid samples, respectively. Glyphosate and AMPA were quantified at 0.105 and 0.210 μg/g (soy protein isolate) and 0.850 and 2.71 μg/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.
Highlights
Glyphosate (N-(phosphonomethyl)glycine) is one of the most widely used broad-spectrum systemic herbicides
The latter were based either on direct analysis by liquid chromatography−diode array detection[15] or liquid chromatography−mass spectrometry (LC-MS)[16−22] or indirect analysis after derivatization followed by gas chromatography−flame photometric detection,[23] gas chromatography−mass spectrometry,[7,24−26] liquid chromatography−fluorescence detection,[8,27−30] or LC-MS.[31−33] Many of these works include laborious cleanup steps involving the use of ion-exchange resins
aminomethylphosphonic acid (AMPA) in nutritional ingredients and products derived from HT crops, as well as in cow’s milk and human breast milk, the present contribution aims to fill this gap of knowledge
Summary
Glyphosate (N-(phosphonomethyl)glycine) is one of the most widely used broad-spectrum systemic herbicides. The analytical approaches available for polar, difficult pesticides, including glyphosate, have been recently reviewed by Raina-Fulton et al.[11] The assay of glyphosate is well established in environmental water analysis.[12−14] limited works have been done in complex food matrices The latter were based either on direct analysis by liquid chromatography−diode array detection[15] or liquid chromatography−mass spectrometry (LC-MS)[16−22] or indirect analysis after derivatization followed by gas chromatography−flame photometric detection,[23] gas chromatography−mass spectrometry,[7,24−26] liquid chromatography−fluorescence detection,[8,27−30] or LC-MS.[31−33] Many of these works include laborious cleanup steps involving the use of ion-exchange resins. Because there are no data on the potential presence and abundance of residues of glyphosate and Received: September 10, 2015 Revised: November 3, 2015 Accepted: November 15, 2015 Published: November 16, 2015
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