Search Results (2,023)

Seed cakes, by-products from the cold press extraction of vegetable oils, are valuable animal feed supplements due to their high content of proteins, carbohydrates, and minerals. However, the presence of anti-nutrients, as well as the rancidification and development of aflatoxins, can impede their intended use, requiring alternative treatment and valorisation methods. Thermal treatment as a procedure for the conversion of seed cakes from walnuts, hemp, pumpkin, flax, and sunflower into valuable products or energy has been investigated in this paper. Thermogravimetry shows the particular behaviour of seed cakes, with several degradation stages at around 230–280 and 340–390 °C, before and after the typical degradation of cellulose. These are related to the volatilisation of fatty acids, which are either free or bonded as triglycerides, and with the thermal degradation of proteins. Torrefaction at 250 °C produced ~75–82 wt% solids, with high calorific values of 24–26 kJ/g and an energy yield above 90%. The liquid products have a complex composition, with most parts of the compounds partitioning between the aqueous phase (strongly dominant) and the oily one (present in traces). The structural components of seed cakes (hemicelluloses, cellulose, and lignin) produce acetic acid, hydroxy ketones, furans, and phenols. In addition to these, most compounds are nitrogen-containing aromatic compounds from the degradation of protein components, which are highly present in seed cakes. Full article

Chronic noncommunicable diseases (NCDs) are responsible for approximately 74% of deaths globally. Medicinal plants have traditionally been used to treat NCDs, including diabetes, cancer, and rheumatic diseases, and are a source of anti-inflammatory compounds. This study aimed to evaluate the anti-inflammatory effects of Rhus trilobata (Rt) extracts and fractions in lipopolysaccharide (LPS)-induced inflammation models in vitro and in vivo. The aqueous extract (RtAE) and five fractions (F2 to F6) were obtained via C18 solid-phase separation and tested in murine LPS-induced J774.1 macrophages. Key inflammatory markers, such as IL-1β, IL-6, TNF-α, and COX-2 gene expression were measured using RT-qPCR, and PGE₂ production was assessed via HPLC-DAD. The in vivo effects were tested in an LPS-induced paw edema model in Wistar rats. Results showed that RtAE at 15 μg/mL significantly decreased IL-1β and IL-6 gene expression in vitro. Fraction F6 further reduced IL-1β, TNF-α, and IL-6 gene expression, COX-2 expression, and PGE₂ production. In vivo, F6 significantly reduced LPS-induced paw edema, inflammatory infiltration, and IL-1β and COX-2 protein expression. Chemical characterization of F6 by UPLC/MS-QTOF revealed at least eight compounds with anti-inflammatory activity. These findings support the anti-inflammatory potential of RtAE and F6, reinforcing the medicinal use of Rt. Full article

The black soldier fly (BSF) Hermetia Illucens can grow rapidly and on a wide variety of organic materials, and it is extensively used as a means of disposing of household organic waste. Different phases of the life cycle of BSF larvae (BSFL) are used in this work to extract chitin after the removal of lipids, mineral salts, and proteins. Multiple techniques, such as X-ray diffractometry, infrared spectroscopy, solid-state Nuclear Magnetic Resonance (¹³C ss-NMR) and thermogravimetric analysis, are used to investigate the chemical and physical characteristics of the extracted samples of chitin, which shows a high degree of acetylation (from 78% to 94%). The extracted chitin shows an increase of the thermal stability of 20 °C in the initial stage of life and 35 °C at the end of the life cycle if compared with a commercial standard. Moreover, the extracted chitin shows an increase in the crystallinity degree during the BSFL growth time (from 72% to 78%). Full article

In this work, aerial parts of Taraxacum officinale F.H. Wigg. produced in Umbria, Italy, were chemically investigated by solid-phase microextraction/gas chromatography–mass spectrometry (SPME/GC-MS) to describe their volatile profile. The results obtained showed the preponderant presence of monoterpenes, with limonene and 1,8-cineole as the main components. Further analyses by GC/MS after derivatization reaction were performed to characterize the non-volatile fraction highlighting the presence of fatty acids and di- and triterpenic compounds. T. officinale methanol and dichloromethane extracts, first analyzed by HRGC/MS, were investigated to evaluate the antioxidant activity, cytotoxicity, and antiproliferative properties of MDA cells on the breast cancer cell line and MCF 10A normal epithelial cells as well as the antioxidant activity by colorimetric assays. The impact on matrix metalloproteinases MMP-9 and MMP-2 was also explored in 3D cell systems to investigate the extracts’ efficacy in reducing cell invasiveness. The extracts tested showed no cytotoxic activity with EC50 > 250 µg/mL on both cell lines. The DPPH assay revealed higher antioxidant activity in the MeOH extract compared with the DCM extract, while the FRAP assay showed a contrasting result, with the DCM extract exhibiting slightly greater antioxidant capacity. After treatment for 24 h with a non-cytotoxic concentration of 500 µg/mL of the tested extracts, gelatin zymography and Western blot analyses demonstrated that both MeOH and DCM extracts influenced the expression of MMP-9 and MMP-2 in MDA cells within the 3D cell model, leading to a significant decrease in the levels of these gelatinases, which are crucial markers of tumor invasiveness. Full article

The preparation of samples for instrumental analysis is the most essential and time-consuming stage of the entire analytical process; it also has the greatest impact on the analysis results. Concentrating the sample, changing its matrix, and removing interferents are often necessary. Techniques for preparing samples for analysis are constantly being developed and modified to meet new challenges, facilitate work, and enable the determination of analytes in the most comprehensive concentration range possible. This paper focuses on using metal-organic frameworks (MOFs) as sorbents in the most popular techniques for preparing liquid samples for analysis, based on liquid-solid extraction. An increase in interest in MOFs-type materials has been observed for about 20 years, mainly due to their sorption properties, resulting, among others, from the high specific surface area, tunable pore size, and the theoretically wide possibility of their modification. This paper presents certain advantages and disadvantages of the most popular sample preparation techniques based on liquid-solid extraction, the newest trends in the application of MOFs as sorbents in those techniques, and, most importantly, presents the reader with a summary, which a specific technique and MOF for the desired application. To make a tailor-made and well-informed choice as to the extraction technique. Full article

Coffee roasting is considered the most critical process in the development of sensory characteristics. During this stage, a substantial number of compounds are generated. Nevertheless, only a limited number of these compounds are responsible for the aroma, referred to as key aroma-active compounds. This study aimed to assess the impact of roasting levels on the formation of these compounds. Coffee was roasted at four different levels: very light (RL85), light (RL75), medium (RL55), and extremely dark (RL25), according to the Specialty Coffee Association (SCA) guidelines. The extraction, olfactory evaluation, and identification of compounds were performed using solid-phase microextraction (SPME), gas chromatography–olfactometry (GC-O), and gas chromatography–mass spectrometry (GC-MS), respectively. A total of 74 compounds were successfully identified, of which 25 were classified as aroma-active compounds. RL75 and RL85 displayed similar aromatic profiles. RL55 was characterized by pleasant notes such as sweet, toasted hazelnut, and caramel. In contrast, RL25 was marked by undesirable odors including burnt notes, putrid, and sulfurous scents. This study is the first to identify key odorant compounds in coffee based on SCA roasting standards. Full article

This study aimed to evaluate the impact of different closures used in second fermentation on the aromatic fraction of sparkling wine. Six types of closures (cork stoppers and screw caps) and 94 months of aging in a bottle were investigated. Headspace solid-phase microextraction (HS-SPME) and thermal desorption (TD) procedures coupled to gas chromatography-mass spectrometry (GCMSMS) analysis were applied. The vectors containing the relative abundance of the volatile compounds are compositional vectors. The statistical analysis of compositional data requires specific techniques that differ from standard techniques. Overall, 101 volatile compounds were identified. HS-SPME extracted the highest percentage of esters, ketones and other compounds, while TD was a useful tool for the obtention of alcohol, acid, ether and alkane compounds. Esters were the most abundant family of compounds. Compositional data analysis, which was applied to study the impact of different closures used in bottle aging after second fermentation on the volatile composition of sparkling wine, concluded that there are differences in the relative abundance of certain volatile compounds between cork stoppers and screw-cap closures. Overall, the most abundant part in screw-cap closures was ethyl hexanoate, and it was ethyl octanoate in cork stoppers. Also, the proportional amount of dimethylamine was higher in screw-cap closures than cork stoppers relative to the entire sample. Full article

Dispersive solid-phase extraction (dSPE) is a crucial step for multiresidue analysis used to remove matrix components from extracts. This purification prevents contamination of instrumental equipment and improves method selectivity, sensitivity, and reproducibility. Therefore, a clean-up step is recommended, but an over-purified extract can lead to analyte loss due to adsorption to the sorbent. This study provides a systematic comparison of the advantages and disadvantages of the well-established dSPE sorbents PSA, GCB, and C18 and the novel dSPE sorbents chitin, chitosan, multi-walled carbon nanotube (MWCNT), and Z-Sep^® (zirconium-based sorbent). They were tested regarding their clean-up capacity by visual inspection, UV, and GC-MS measurements. The recovery rates of 98 analytes, including pesticides, active pharmaceutical ingredients, and emerging environmental pollutants with a broad range of physicochemical properties, were determined by GC-MS/MS. Experiments were performed with five different matrices, commonly used in food analysis (spinach, orange, avocado, salmon, and bovine liver). Overall, Z-Sep^® was the best sorbent regarding clean-up capacity, reducing matrix components to the greatest extent with a median of 50% in UV and GC-MS measurements, while MWCNTs had the largest impact on analyte recovery, with 14 analytes showing recoveries below 70%. PSA showed the best performance overall. Full article

Vanadium (V) was successfully extracted from a high phosphorus vanadium residue (HPVR) through a carbonation process. Vanadium within HPVR substitutes for Fe in the mineral structure of Ca₉(Fe,V)(PO₄)₇ at elevated temperatures, Na₂CO₃ reacts with V to form sodium metavanadate (NaVO₃), concurrently generating calcium carbonate (CaCO₃) through its interaction with Ca₉(Fe,V)(PO₄)₇. Subsequently, V is liberated and leached by water, dissolving in the aqueous phase as metavanadate ions (VO³⁻). Crucial factors influencing V leaching efficiency include roasting time, roasting temperature, and the amount of Na₂CO₃ utilized. Response Surface Methodology (RSM) was employed. The optimized parameters determined were as follows: a roasting temperature of 850 °C, a roasting duration of 120 min, a Na₂CO₃ dosage of 8.01%, a liquid-to-solid ratio (L/S) of 3, and a leaching time of 60 min. Under these conditions, a remarkable V leaching efficiency of 83.82% was achieved. This study underscores the viability of a simplified approach for treating solid waste containing metal slag, which not only mitigates environmental pollution but also yields valuable metals. Full article

Quinolone antibiotics (QNs) contamination in the aquatic environment is a global public health issue considering their resistance and mobility. In this study, a simple, efficient, and sensitive method was developed for the accurate quantification of fifteen QNs in water using automated disk-based solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). By utilizing a 3M SDB-XC disk to enrich QNs from a 1000 mL water sample, the detection limits were improved to 0.008–0.055 ng/L due to the satisfactory enrichment factors of 897−1136, but only requiring about 60 min per six samples. The linearity of the method ranged from 0.05 to 100 μg/L for the 15 QNs, with correlation coefficients of 0.9992–0.9999, and the recoveries were in the range of 81–114%, with relative standard deviations of 0.2–13.3% (n = 6). The developed method was applicable for the quantification of trace QNs at low ng/L levels in drinking and environmental waters. The results showed that no QNs were detected in tap water, while three and four QNs were detected in the river water of Zhoushan and the seawater of Daiquyang and Yueqing Bay, East China, respectively, with a total concentration of 1.600–8.511 ng/L and 1.651–16.421 ng/L, respectively. Among the detected QNs, ofloxacin (OFL) was the predominant compound in river water, while enrofloxacin (ENR) was predominant in seawater. The risk quotient (RQ) results revealed that QNs posed a low risk to crustaceans and fish, but a low-to-medium risk to algae, and OFL presented the main ecological risk factor in river water, while ENR and CIP in seawater. Overall, the proposed automated disk-based SPE–UPLC–MS/MS method is highly efficient and sensitive, making it suitable for routine analysis of QNs in drinking and environmental waters. Full article

The fruit of the date tree (Phoenix dactylifera L.) is increasingly recognized for its nutritional and functional value. This exotic fruit shows variable composition, influenced by factors such as variety, ripening stage, and climatic conditions. In this context, this study aimed to investigate the nutritional profile and the bioactive components, including phenolic compounds and oligosaccharides, in different varieties of dates from Saudi Arabia collected at the Tamr ripening stage. The HPLC-ESI-MS analysis identified a total of 15 phenolic compounds, principally phenolic acids and flavonoids. Among the varieties tested, Safawi exhibited the highest phenolic concentration (1132 µg/100 g dw). To the best of our knowledge, the oligosaccharide composition is described for the first time among different varieties, with Sukari showing the highest concentration (3.37 g/100 g dw). Moreover, the antioxidant capacity (DPPH, ABTS, and FRAP assays) was assessed following a solid-phase extraction (SPE) clean-up to remove interferents, especially sugars. These results provide valuable insights into the health-promoting properties of date fruit as a functional food and provide a foundation for further research into their industrial applications as functional ingredients. Full article

As a traditional Chinese medicine (TCM), Allii Macrostemonis Bulbus (AMB) is a key herb for the treatment of thoracic paralytic cardiac pain, but its quality evaluation method has not yet been fully clarified. In this study, chromatographic fingerprints of AMB were developed using solid-phase extraction–high-performance liquid chromatography–evaporative light scattering detection (SPE-HPLC-ELSD) to evaluate the quality of AMB from various origins and processing methods. This was achieved by employing chemical pattern recognition techniques and verifying the feasibility and applicability of the quality evaluation of AMB through the quantitative analysis of multi-components via a single-marker (QAMS) method. Through the analysis of the fingerprints of 18 batches of AMB, 30 common peaks were screened, and 6 components (adenosine, syringin, macrostemonoside T, macrostemonoside A, macrostemonoside U, and macrostemonoside V) were identified. Moreover, three differential markers (macrostemonoside A, macrostemonoside T, and macrostemonoside U) were screened out using chemometrics techniques, including principal component analysis (PCA), hierarchical cluster analysis (HCA), and orthogonal partial least squares discriminant analysis (OPLS-DA). Subsequently, a QAMS method was established for macrostemonoside T and macrostemonoside U using macrostemonoside A as an internal reference. The results demonstrate the method’s accuracy, reproducibility, and stability, rendering it suitable for the quality evaluation of AMB. This study provides a theoretical basis for drug quality control and the discovery of quality markers for AMB. Full article

Rifaximin and rifampicin are good broad-spectrum antimicrobials. The irrational use of antimicrobial drugs in veterinary clinics could threaten public health and food safety. It is necessary to develop a reliable detection method of the residue for enhancing the rational supervision of the use of such drugs, reducing and slowing down the generation of bacterial resistance, and promoting animal food safety and human health. So, this study developed an LC-MS/MS method for the detection of rifaximin and rifampicin residues in animal-origin foods. The residual rifaximin and rifampicin of homogenized test materials were extracted with acetonitrile-dichloromethane solution or acetonitrile in the presence of anhydrous sodium sulfate and vitamin C, purified by dispersible solid phase extraction, determined by LC-MS/MS, and quantified by the internal standard method. The specificity, sensitivity, matrix effect, accuracy, and precision of the method were investigated in the edible tissues of cattle, swine, or chicken. In addition, the stability of the standard stock solution and the standard working solution was also investigated. The method was suitable for the muscle, liver, kidney, fat, milk, and eggs of cattle, swine, or chicken, as well as fish and shrimp. The specificity of the method was good, and the detection of the analytes was not affected by different matrices. Both the LOD and LOQ of the two analytes were 5 μg/kg and 10 μg/kg, respectively. The results of matrix effects in each tissue were in the range of 80–120%; there were no significant matrix effects. The average accuracy of rifaximin and rifampicin in different foodstuffs of animal origin was between 80% and 120%, and the method precision was below 20% (RSD). The proposed method showed good performance for determination, which could be employed for the extraction, purification, and detection of residual rifaximin and rifampicin in edible animal tissues. The pretreatment procedure of tissue samples was simple and feasible. The method was highly specific, stable, reliable, and with high sensitivity, accuracy, and precision, which met the requirements of quantitative detection of veterinary drug residues. Full article

Fusarium graminearum (F. graminearum) in maize poses a threat to grain security. Current non-destructive detection methods face limited practical applications in grain quality detection. This study aims to understand the optical properties and volatileomics of F. graminearum-contaminated maize. Specifically, the transmission and reflection spectra (wavelength range of 200–1100 nm) were used to explore the optical properties of F. graminearum-contaminated maize. Volatile organic compounds (VOCs) of F. graminearum-contaminated maize were determined by headspace solid phase micro-extraction with gas chromatography-tandem mass spectrometry. The VOCs of normal maize were mainly alcohols and ketones, while the VOCs of severely contaminated maize became organic acids and alcohols. The ultraviolet excitation spectrum of maize showed a peak redshift as fungi grew, and the intensity decreased in the 400–600 nm band. Peak redshift and intensity changes were observed in the visible/near-infrared reflectance and transmission spectra of F. graminearum-contaminated maize. Remarkably, optical imaging platforms based on optical properties were developed to ensure high-throughput detection for single-kernel maize. The developed imaging platform could achieve more than 80% classification accuracy, whereas asymmetric polarization imaging achieved more than 93% prediction accuracy. Overall, these results can provide theoretical support for the cost-effective preparation of low-cost gas sensors and high-prediction sorting equipment for maize quality detection. Full article

This study investigates the effect of prolonged maceration, pre-fermentation heating, and barrel aging on the volatile aroma profile and sensory characteristics of Teran wine. The vinification processes included a control treatment (7-day maceration, TM7-Y; Y—young wine), 10-day maceration (TM10-Y), 21-day post-fermentation maceration (TM21-Y), and 48-h pre-fermentation heating at 45 °C followed by 8-day maceration (TPHT-Y). All wines were then aged in oak barrels for six months, resulting in TM7-A, TM10-A, TM21-A, and TPHT-A wines (A—aged wine). Volatile compounds were extracted using headspace solid-phase microextraction (HS-SPME) and analyzed by gas chromatography/mass spectrometry (GC/MS), while sensory profiles were evaluated using quantitative descriptive analysis (QDA). TPHT-Y and TM21-Y treatments reduced several groups of free volatile compounds while enhancing sensory properties, with TM21-Y wines notably exhibiting pronounced dried fruit notes, likely due to high β-damascenone concentrations. Conversely, TM10-Y and TM7-Y treatments resulted in significantly higher concentrations of the most volatile aroma compounds. Aging in oak barrels significantly increased the levels of particular free volatile compounds like C₁₃-norisoprenoids, volatile phenols, furans, and lactones. It also enhanced sensory quality, with fruity aromas prominent across all treatments, and TM21-A and TPHT-A wines showing strong dried fruit, jam, and liqueur notes. This study offers valuable insights into tailoring wine aromas and sensory attributes through specific vinification techniques, contributing to a more refined approach to optimizing wine production. In conclusion, the findings highlight the importance of maceration and aging techniques in developing complex and desirable wine profiles, offering practical guidance for improving Teran wine quality. Full article