As a widely consumed foodstuff, milk and dairy products are increasingly studied over the years. At the present time, milk profiling is used as a benchmark to assess the properties of milk. Modern biomolecular mass spectrometers have become invaluable to fully characterize the milk composition. This review reports the analysis of milk and its components using liquid chromatography coupled with mass spectrometry (LC–MS). LC–MS analysis as a whole will be discussed subdivided into the major constituents of milk, namely, lipids, proteins, sugars and the mineral fraction.

The 2,2-diphenyl-1-picrylhydrazyl (DPPH•) assay is widely used to determine the antioxidant activity of food products and extracts. However, the common DPPH• protocol uses a two-point measurement and does not give information about the kinetics of the reaction. A novel stoichio-kinetic model applied in this study monitors the consumption of DPPH• by common antioxidants following the second order reaction. The fitting of such decay yields the rate constant k₁, which describes the main reaction between antioxidants and DPPH•, and the rate constant k₂, which is attributed to a slower side reaction considering the products generated between the transient radicals (AO•) and another molecule of DPPH•. The model was first applied to antioxidant standards. Sinapic acid, Trolox and ascorbic and chlorogenic acids did not show any side reaction. Instead gallic, ferulic and caffeic acids achieved the best fitting with k₂. The products of the side reaction for these compounds were confirmed and identified with high-resolution mass spectrometry. Finally, the kinetic model was applied to evaluate the antioxidant activity of eight herbal extracts. This study suggests a new kinetic approach to standardize the common DPPH• assay for the determination of antioxidant activity.

Hay milk is a traditional dairy product recently launched on the market. It is protected as “traditional specialty guaranteed” (TSG) and subjected to strict regulations. One of the most important restrictions is that the cow’s feed ration must be free from silage. There is the need for analytical methods that can discriminate milk obtained from a feeding regime including silage. This study proposes two analytical approaches to assess the authenticity of hay milk. Hay milk and milk from cows fed either with maize or grass silage were analyzed by targeted GC-MS for cyclopropane fatty acid (dihydrosterculic acid, DHSA) detection, since this fatty acid is strictly related to the bacterial strains found in silage, and by HPLC-HRMS. The presence of DHSA was correlated to the presence of maize silage in the feed, whereas it was ambiguous with grass silage. HPLC-HRMS analysis resulted in the identification of 14 triacylglycerol biomarkers in milk. With the use of these biomarkers and multivariate statistical analysis, we were able to predict the use of maize and grass silage in the cow’s diet with 100% recognition. Our findings suggest that the use of analytical approaches based on HRMS is a viable authentication method for hay milk.

This research paper investigates the use of 5-hydroxymethylfurfural (5-HMF) as marker for the heat treatment of spreadable dairy creams (dulce de leche, DL). The proposed method applies solid-phase extraction (SPE) with final analysis by liquid chromatography coupled with high-resolution mass spectrometry (SPE-LC–MS). The method was successfully applied to analyze spreadable dairy creams prepared by hot melt extrusion using different heating temperatures from 100 to 130 °C. The concentrations of 5-HMF correlated linearly with the applied temperatures, with a signal response in the range from 0.5 to 100 μM (R² = 0.9997). The limit of detection (LOD) was 1.54 ± 0.03 µM with a precision of 1.77%. The results were compared with the analysis of 5-HMF in spreadable dairy creams using reference methods for the determination of 5-HMF in milk products. These methods mainly employed acid digestion and derivatization as pre-processing steps and determined 5-HMF spectrophotometrically and via HPLC–UV. These resulted in higher LOD (2.99 and 2.01 μΜ) and less precision (4.44 and 2.09%) compared to the proposed method. Furthermore, the proposed pre-processing procedure was faster by omitting the acid digestion and derivatization steps and by employing SPE.

Vitis vinifera L. ‘Gewürztraminer’ produces distinctive, aromatic wines that are strongly influenced by their terroir. This metabolomic study used a data-driven approach, including Principal Component Analysis (PCA) and Multifactorial Analysis (MFA), to correlate a quali-quantitative multivariate concept of terroir (including soil characteristics, and altitude) with sensory, phenolic, antioxidant, and volatile profiles of wines. The study analyzed wines from seven ‘Gewürztraminer’ vineyards, chosen to minimize the variability due to climate differences. Based on the soil data, the vineyards were clustered into two distinct groups: clay silicate (Group A) and dolomitic (Group B) soils. Group A exhibited lower levels of aromatic compounds such as linalool and higher levels of phenolic compounds such as gallocatechin than Group B. These findings indicate that even small changes in terroir within the same region can significantly impact the chemical, functional (antioxidant), and sensory properties of ‘Gewürztraminer’ wines, highlighting the importance of terroir in wine production. Statistical analyses confirmed the significance of these correlations (p < 0.05), highlighting the need for further research into the intricate relationship between terroir and wine quality.