User-friendly platform for analysis of high mass intact proteins and glycopeptides by laser desorption/ionization-mass spectrometry based on copper oxide particles.

Matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS) based on micro/nanostructured materials with different natures has received increasing attention for the analysis of a wide variety of analytes. However, up to now, only a few studies have shown the application of simple platforms in MALDI-MS for the identification of intact proteins. The present work reports on the application of copper oxide particles (Cu2O PS), obtained by a greener route, in combination with low amounts of 2,5-dihydroxybenzoic acid (DHB) as a novel hybrid platform. The combined Cu2O PS@DHB matrix, containing only 2.5 mg mL-1 of particles and 10 mg mL-1 of DHB, was easily applicable in MALDI-MS without surface modification of target plates. Under optimal conditions, the analysis of intact proteins up to 150,000 Da was possible, including immunoglobulin G, bovine serum albumin, and cytochrome C with adequate spot-to-spot signal reproducibility (RSD < 10%). In addition, the analysis of glycopeptides from IgG digests was carried out to prove the multipurpose application of the Cu2O PS@DHB platform in the low m/z range (2500-3000 Da). From the obtained results, it can be concluded that the optical and surface properties of as-synthesized Cu2O PS are likely to be responsible for the superior performance of Cu2O PS@DHB in comparison with conventional matrices. In this sense, the proposed user-friendly methodology opens up the prospect for possible implementation in bioanalysis and diagnostic research.

Combining capillary electrophoresis and chemometric tools for the straightforward determination of imidazolinone herbicides in plant-based milks.

BACKGROUND: Highly polar herbicides, such as imidazolinones, are used for weed control to increase agricultural productivity and crop quality. However, their misapplication can lead to residues in ready-to-eat food with a potential health risk for consumers. Hence, the fast determination of these herbicides is necessary for timely action. In this work, an eco-friendly method based on capillary zone electrophoresis combined with chemometrics was used for the determination of imazapyr and imazamox in vegetable-based beverages such as soy and quinoa milk. RESULTS: The analytical strategy consisted of only three steps: (i) protein precipitation prior to sample injection (ii) data pre-processing to reduce the background and make corrections on electrophoretic times shift, and (iii) resolution of fully overlapped capillary electrophoresis (CE) peaks by the well-known partial least square (PLS) algorithm, which extracts quantitative information attributed to the analytes. The method was successfully applied in the concentration range between 1.00 and 100 µg L-1 with coefficient of determination of the calibration (R2 cal) and prediction (R2 pred) > 0.90, residual prediction deviation of calibration (RPDcal) and of prediction (RPDpred) > 3, and relative error of prediction (REP) > 11 in the analyzed sample matrices, in the three built methods (quinoa samples, soy samples, and joint quinoa and soy samples). CONCLUSION: The proposed methodology offers a simple and quick alternative for determining imidazolinones at trace concentrations in vegetable beverages, such as quinoa and soy milk, without complex sample preparation. The results were consistent with those obtained using more complex techniques, confirming the applicability of this method. © 2024 Society of Chemical Industry.

Microwave-assisted synthesis of copper oxide particles and its application for determination of imazapyr in environmental samples.

Imazapyr (IMA) is currently applied as pre- and post-emergence herbicide for control of weeds in crops. Because of its extensive use, IMA residues may reach water sources and soils. Consequently, its accurate measurement is demanded for timely actions with minimal involved steps and analysis time. Herein, copper oxide particles (Cu2O PS) were proposed as chemical sensor for determination of IMA residues. Cu2O PS were prepared by a facile microwave-assisted method using glucose as reducing agent and polyvinylpyrrolidone as stabilizer. The effect of main experimental parameters on the conversion rate of the Cu2O PS were analyzed by the response surface methodology. Obtained particles were thoroughly characterized in order to determine the particle size distribution, morphology, surface charge, optical and surface properties for further application. Determination of IMA was only based on the localized surface plasmon resonance band of Cu2O PS at 473 nm. Under optimal conditions, the method was evaluated in the concentration range between 80.0 and 1,000 µg L-1 showing a limit of detection about 101 µg L-1 (R2 >0.98). The applicability of the proposed methodology to determine IMA in soil and water samples was assessed with satisfactory recoveries (104-121.8%) displaying a good implementation prospect in environmental complex matrices.