Unravelling the combined impacts of drought and Cu in barley plants - double trouble?

The occurrence of drought in soils, particularly in those contaminated by metals, poses a current threat to crops, as these factors can interact and induce unique stress responses. Therefore, this study mainly focused on understanding the crosstalk between drought and copper (Cu) stress in the physiology of the barley (Hordeum vulgare L.) plant. Using a bifactorial experimental design, seedlings were grown in a natural soil under the following treatments: plants continuously irrigated in uncontaminated soil for 14 days (control); plants continuously irrigated in Cu-contaminated soil (115 mg Cu kg-1) for 14 days (Cu); plants only irrigated during the initials 7 days of growth in uncontaminated soil (drought); plants co-exposed to Cu and drought (combined). After 14 days of growth, the results revealed that drought prevented Cu bioaccumulation in barley roots, which were still severely affected by the metal, both individually and in combination with the water deficit. Furthermore, individual and combined exposure to these stressors resulted in impaired photosynthetic performance in barley plants. Despite the increased activation of enzymatic and non-enzymatic antioxidant defence mechanisms, particularly in the green organs, the plants co-exposed to both stress factors still showed higher oxidative damage, severely impacting biomass production.

Untargeted metabolomic profiling of fresh and dried leaf extracts of young and mature Eucalyptus globulus trees indicates differences in the presence of specialized metabolites.

Aqueous extracts from Eucalyptus globulus leaves contain a wide variety of specialized metabolites, mainly polyphenols and appreciable amounts of volatile compounds, which are responsible for their diverse biological activities, such as antioxidant, antimicrobial, and allelopathic features. For this reason, several studies have been conducted to explore the composition of E. globulus leaf extracts for multiple therapeutic and commercial applications. However, so far, the available bibliographic reports only refer to the chemical composition of extracts prepared with leaves from mature trees, leaving much to clarify about the composition of juvenile eucalyptus leaf extracts. Furthermore, there is no consensus regarding the type of leaves, fresh or dried ones, to be used in the extraction procedure, considering the highest recovery of biologically active compounds. In this sense, this study aimed to characterize the chemical composition of aqueous extracts prepared with fresh and dried leaves from young and mature E. globulus trees. For this, leaf biomass from young and mature E. globulus trees was collected in three distinct places from a forest area, and after oven-drying a portion of the leaves, an extraction in hot water was carried out, followed by GC-MS and HPLC-MS/MS analyses. The results revealed that the maturity of eucalyptus trees and biomass drying significantly influenced the volatile and non-volatile composition of the aqueous extracts. Accordingly, while fresh leaf extracts of young trees had great levels of hydrolysable tannins, extracts prepared with fresh leaves from mature trees presented a wide range of terpenes. When dried leaf material was used, extracts had notorious contents of amino acids derivatives, C13 norisoprenoids, fatty and other organic acids. Overall, this study showed, for the first time, that plant maturity (young vs mature) and pre-processing (fresh vs dried) of foliar biomass of E. globulus trees need to be considered in the preparation of leaf aqueous extracts depending on the desired purposes, since major changes in what regards biologically active compounds were found.

Recent advances in salt-assisted LLE for analyzing biological samples.

Salt-assisted LLE (SALLE) has been attracting growing interest in bioanalysis. The technique is particularly advantageous due to its simple and fast experimental execution using conventional laboratory equipment. Besides, SALLE uses water-miscible organic solvents making the extracts readily compatible with various analytical separation and detection techniques. This article presents a brief overview of the extraction technique and its role in bioanalysis. Some of the most relevant achievements on SALLE application to biological samples are discussed - namely the study of the main extraction parameters, the combination with other extraction techniques and the instrumental analysis of the extracts. Developments on automation, miniaturization and microextraction for SALLE procedures are also discussed as a perspective for future applications even more attractive for the analysis of biological samples.

Analysis of biogenic amines in wines by salting-out assisted liquid-liquid extraction and high-performance liquid chromatography with fluorimetric detection.

Biogenic amines are nitrogenous organic compounds of low molecular weight that are either formed or metabolized in cells of living organisms and can be found in several food products, being produced mainly by amino acid decarboxylation. When ingested in high concentrations they can induce several health problems in humans. In alcoholic beverages, and especially in wine, they are formed during the vinification process as a result of the action of microorganisms. In this work it is proposed a new methodology for the determination of biogenic amines in wines, which includes a sample preparation approach based on salting-out assisted liquid-liquid extraction, the use of dansyl chloride for the derivatization and chromatographic separation by high-performance liquid chromatography with fluorimetric detection. The salting-out effect is used to promote phase separation between water and a water-miscible organic solvent, while improving the extraction of organic or inorganic species. Several extraction parameters were optimized, such as the dansyl chloride concentration, pH and the effects caused by the order in which the extraction and derivatization were performed. Extraction of amines, and consequent detection, depends on the presence of dansyl chloride in solution prior to extraction. The results showed the possibility to simultaneously perform the extraction and the derivatization, making sample preparation easier and less time-consuming. The methodology was successfully applied to the determination of biogenic amines in five wines (white, red and rosé). This method has the potential to be a good alternative to existing methods since it is cheaper, easier and simplifies the sample preparation step.

An overview on cardamonin.

Cardamonin, as shown by the increasing number of publications, has received growing attention from the scientific community due to the expectations toward its benefits to human health. In this study, research on cardamonin is reviewed, including its natural sources, health promoting aspects, and analytical methods for its determination. Therefore, this article hopes to aid current and future researchers on the search for reliable answers concerning cardamonin's value in medicine.

Another glimpse over the salting-out assisted liquid-liquid extraction in acetonitrile/water mixtures.

The use of the salting-out effect in analytical chemistry is very diverse and can be applied to increase the volatility of the analytes in headspace extractions, to cause the precipitation of proteins in biological samples or to improve the recoveries in liquid-liquid extractions. In the latter, the salting-out process can be used to create a phase separation between water-miscible organic solvents and water. Salting-out assisted liquid-liquid extraction (SALLE) is an advantageous sample preparation technique aiming HPLC-UV analysis when developing analytical methodologies. In fact, some new extraction methodologies like QuEChERS include the SALLE concept. This manuscript discusses another point of view over SALLE with particular emphasis over acetonitrile-water mixtures for HPLC-UV analysis; the influence of the salting-out agents, their concentration and the water-acetonitrile volume ratios were the studied parameters. α-dicarbonyl compounds and beer were used as test analytes and test samples, respectively. The influence of the studied parameters was characterized by the obtained phase separation volume ratio and the fraction of α-dicarbonyls extracted to the acetonitrile phase. Results allowed the distribution of salts within three groups according to the phase separation and their extractability: (1) chlorides and acetates, (2) carbonates and sulfates and (3) magnesium sulfate; of all tested salts, sodium chloride had the highest influence on the α-dicarbonyls fraction extracted.

Gas-diffusion microextraction.

Gas-diffusion microextraction (GDME) is an innovative technique that combines the advantages of membrane-aided gas-diffusion with microextraction concepts. GDME makes uses of a novel portable and low-cost device that comprises a small, commercially available, semi-permeable membrane. Furthermore, if derivatization is integrated into the GDME concept, considerable enrichment factors can be obtained. It may become a powerful tool for any analyst who intends to quantify volatile and semi-volatile analytes in various kinds of matrices. The analysis of vicinal diketones in beer was used as a case study to show GDME applicability and capabilities. Vicinal diketones were derivatized with o-phenylenediamine and then determined by HPLC-UV. Obtained results showed good repeatability and precision with extraction periods at the minute time span.

Analysis of aldehydes in beer by gas-diffusion microextraction: characterization by high-performance liquid chromatography-diode-array detection-atmospheric pressure chemical ionization-mass spectrometry.

In this work, a recently developed extraction technique for sample preparation aiming the analysis of volatile and semi-volatile compounds named gas-diffusion microextraction (GDME) is applied in the chromatographic analysis of aldehydes in beer. Aldehydes-namely acetaldehyde (AA), methylpropanal (MA) and furfural (FA)-were simultaneously extracted and derivatized with 2,4-dinitrophenylhydrazine (DNPH), then the derivatives were separated and analyzed by high-performance liquid chromatography with spectrophotometric detection (HPLC-UV). The identity of the eluted compounds was confirmed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass-spectrometry detection in the negative ion mode (HPLC-APCI-MS). The developed methodology showed good repeatability (ca. 5%) and linearity as well as good limits of detection (AA-12.3, FA-1.5 and MA 5.4microgL(-1)) and quantification (AA-41, FA-4.9 and MA 18microgL(-1)); it also appears to be competitive in terms of speed and cost of analysis.

Development of a membraneless extraction module for the extraction of volatile compounds: application in the chromatographic analysis of vicinal diketones in beer.

A membraneless extraction module (MLEM) for the sample preparation of volatile compounds and its use for the chromatographic analysis of vicinal diketones in beer are reported. The extraction process is based on the same principles of gas diffusion (GD) and pervaporation (PV); however it does not use a membrane. This module has a lower chamber where the sample continuously flows, while volatile compounds evaporate to the headspace. Inside the module there is a suspended small reactor, where a small volume of a suitable acceptor solution is placed. This extraction module was tested in the determination of vicinal diketones (VDKs) in beer (CV=5%; LOD=4 microg L(-1)), showing applicability with real samples. Several parameters of the extraction process, such as temperature, sample flow and extraction time, were studied and optimized. This module proved to be a good tool for the sampling of volatile compounds, since the extraction is made without using a membrane avoiding all the robustness problems related with its use.