The major components of industrial thin (SSL) and thick (THSL) liquors from acidic magnesium–based sulphite pulping of Eucalyptus globulus wood have been characterized. The analysis of sugars in SSL revealed the predominance of xylose, which was present in the form of sugar monomer (ca. 70%) and as xylo-oligosaccharides (ca. 30%). Lignosulphonates (LS) were the most abundant organic fraction of spent liquor (ca. 50% of liquor dry matter) consisting of sulphonated oligomers (SO₃H ≈ 20% w/w) of low molecular weight (Mw ≈ 1000–1300 Da) and constituted mainly by syringyl units (syringyl:guaiacyl ratio = 81:19). The major phenolic extractives of THSL were pyrogallol (93 g/ton) and gallic acid (1020 g/ton), and the most abundant fatty acid and sterol were tetracosanoic acid (6 g/ton) and β -sitosterol (45 g/ton), respectively. The structural changes of macromolecular components during the liquor evaporation were discussed.

The structure of lignosulphonates (LS) from acidic magnesium-based sulphite pulping of Eucalyptus globulus wood has been studied. LS from thin and thick spent liquors were purified by dialysis and characterised by 1D/2D Nuclear Magnetic Resonance (NMR) and Electrospray Ionization Mass Spectrometry (ESI-MS). It was suggested that major part of LS is comprised of partially sulphonated low molecular weight oligomers formed via extensive cleavage of β-O-4 bonds in eucalypt lignin upon sulphite pulping. More than ten types of LS structures derived from different lignin structural units have been identified. A significant proportion of LS (> 20%) is comprised by monomeric compounds, mainly 4-allyl-2,6-dimethoxyphenyl-α -sulphonic and 4-propyl-2,6-dimethoxyphenyl-α,γ -disulphonic acids. LS revealed partial degradation during the thin liquor evaporation leading to cleavage of ether and carbon-carbon linkages in the side chain and to the increasing of the condensation degree.

Agricultural by-products are often hidden sources of healthy plant ingredients. The investigation of the nutritional values of these by-products is essential towards sustainable agriculture and improved food systems. In the vine industry, grape leaves are a bulky side product which is strategically removed and treated as waste in the process of wine production. In this work we performed an untargeted metabolomic profiling of the methanol extract of the leaves of Vitis vinifera cultivar ‘Pinot noir’, analysed their fatty acid content, and estimated their antioxidative capacity, with the purpose of investigating its nutritional and medicinal value. Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) analysis identified the presence of numerous compounds which are known to possess diverse nutritional and pharmacological properties, particularly polyphenols and phenolic compounds (e.g. caffeic acid, catechin, kaempferol and quercetin), several phytosterols and fatty acids. Fatty acids were the most represented lipids’ secondary class, with the essential alpha-linolenic acid being the most abundant in ‘Pinot noir’ leaves, with a relative content of 42%. Also, we have found that ‘Pinot noir’ leaves present a high antioxidant capacity, putting grapevine leaves at the top of the list of foods with the highest antioxidative activity. Our findings scientifically confirmed that ‘Pinot noir’ leaves have a high content and diversity of biologically active phytochemical compounds which make it of exceptional interest for pharmaceutical and food industries.

In metabolomics there is an ever-growing need for faster and more comprehensive analysis methods to cope with the increase of biological studies. Direct infusion Fourier-transform ion cyclotron-resonance mass spectrometry (DI-FTICR-MS) is used in non-targeted metabolomics to obtain high-resolution snapshots of the metabolic state of a system. In any metabolic profiling study, the establishment of an effective metabolite extraction protocol is paramount. We developed an improved metabolite extraction method, compatible with DI-FTICR-MS-based metabolomics, using grapevine leaves. This extraction protocol allowed the extraction of polar and non-polar compounds, covering all major classes found in plants and increasing metabolome coverage.