Polar pesticide analyses : validation of glyphosate determination in soil by LC-MS/MS

Although glyphosate is a heavily applied herbicide worldwide, the risk of environmental contamination through transport mechanisms of this substance is still not well documented and the methods for its analysis are usually very complex and nor sensitive enough. In the measurement procedure with LC-MS/MS, a negative mode was used. FMOC-Cl derivatized glyphosate ions were identified by the precise determination of their ion mass. The LOQ was 0.01 mg/kg, with recovery of 101.4±4.49% and linearity over 0.99. The obtain method demonstrates the sensitivity, which enables measurements of glyphosate soil as a matrix. The success of the new extraction method was confirmed by measuring spiked soil samples to control recovery, linearity, LOD and LOQ

Detection of glyphosate and its metabolite aminomethylphosphonic acid: Risk assessment for the aquatic organisms

This paper delves into a thorough risk assessment of glyphosate, a widely used herbicide, and its metabolite, aminomethylphosphonic acid (AMPA), within the aquatic ecosystems of the Danube-Tisa-Danube (DTD) network, which represents large land drained system between Serbia, Hungary, and Romania. The primary objective is to employ a Toxicity and Exposure Ratio (TER) framework, encompassing both acute and chronic considerations, to comprehensively evaluate the potential risks these agrochemicals pose to aquatic organisms in the intricate hydro system of the DTD. The study integrates field data, laboratory experiments, and mathematical modeling to quantify glyphosate and AMPA exposure levels in the DTD channels. Furthermore, it explores the toxicological impacts of these substances on a diverse range of aquatic organisms, such as fish, invertebrates, and amphibians, considering acute effects arising from short-term exposure and chronic effects resulting from prolonged interactions. This research aims to provide a holistic understanding of the risk landscape associated with glyphosate and AMPA in the DTD hydro system by employing the TER approach. The findings contribute valuable insights into the potential ecological implications of herbicide usage in this critical water network, aiding regulatory decision-making and facilitating the development of targeted mitigation strategies to safeguard aquatic biodiversity and ecosystem health

Method Validation for the Determination of Glyphosate and Aminomethylphosphonic Acid in Water by LC-MS/MS

The massive use of glyphosate as a herbicide compound has led to the ubiquity of AMPA in the environment, especially in water. So, the present work aimed to establish the validation parameters of the LC-MS/MS method for glyphosate and its metabolite AMPA, determination in water. During the extraction process the derivatization of glyphosate as an extreme polar pesticide, was done using FMOC. The validation results show that the method met the criteria given in SANTE/11312/2021 for all the investigated validation parameters as well as estimated measurement uncertainty

Determination of ergot alkaloids in buckwheat flour by liquid chromatography coupled to tandem mass spectrometry

The study aimed to analyze the ergot alkaloid profile in buckwheat flour using the LC-MS/MS method. This method proved effective for quantifying six ergot alkaloids: ergocornine, ergocristine, ergometrine, ergosine, ergotamine, α-ergocryptine, and their epimers. It reliably detected these alkaloids at levels as low as 10 µg/kg. The procedure involved extracting the alkaloids with a mixture of methanol and water containing 0.4 % formic acid, followed by UHPLC-MS/MS analysis. The method demonstrated high sensitivity, accuracy, and precision. The study analyzed 30 buckwheat flour samples from the Serbian market. Among these, 29 samples showed no detectable ergot alkaloids. However, one sample tested positive for five ergot alkaloids, albeit within the proposed Maximum Residue Level (MRL) limits