Evaluation of High Vacuum Flavor Extraction Device as a Novel Technique for the Extraction of Volatile Compounds.

In this study, a high vacuum flavor extraction (HVE) device was developed to address the limitations of traditional extraction methods, such as extended extraction times and artifact generation during high-temperature processes. Firstly, the repeatability and precision of the HVE method were evaluated through quantitative analysis of twelve volatile odor compounds across seven replicate extractions using gas chromatography-flame ionization detection (GC-FID). The results showed that the HVE system achieved a mean relative standard deviation (RSD) of 11.60 ± 1.79% and a recovery rate of 90.55 ± 4.56%, demonstrating its precision and reproducibility. Secondly, the performance of HVE was compared with solvent-assisted flavor evaporation (SAFE) and simultaneous distillation-extraction (SDE) for extracting flavor compounds from fried tilapia mince. The results indicated that HVE was more effective, particularly in extracting aldehydes and pyrazines, which are key contributors to the flavor profile. Finally, sensory evaluations supported these findings, showing that the odor profiles obtained through HVE were most similar to the original sample, with a similarity score of 72.55%, compared to 69.25% for SAFE and 60.29% for SDE. These findings suggest that HVE is a suitable method for the extraction and analysis of volatile compounds in complex food matrices such as fried tilapia mince.

Unveiling the hidden potential: Above-ground parts of Paris yunnanensis Franch. Is promise as an anti-acne therapeutic beyond traditional medicinal sites.

The dried rhizomes of Paris yunnanensis Franch. have been extensively utilized in traditional Chinese medicine as hemostatic, antitumor, and antimicrobial agents. An examination of classical texts and renowned Chinese medical formulations showcased its efficacy in acne treatment. Presently, there is a significant scarcity of Paris resources. Consider directing attention towards the non-medicinal parts of Paris to mitigate the strain on medicinal resources within this realm. To address these resource limitations, this study investigated the bioactivity and pharmacodynamics of the above-ground parts of Paris (AGPP). A synergistic approach integrating network pharmacology, molecular docking (in silico validation), and animal experimentation (in vivo validation) was employed to elucidate the potential mechanisms underlying the efficacy of AGPP against acne vulgaris in this study. The active constituents in AGPP extracts were identified via UHPLC-Q-Orbitrap HRMS analysis, with their targets extracted for network pharmacological analysis. KEGG pathway analysis unveiled potential therapeutic mechanisms, validated through molecular docking and rat auricular acne model experiments. Comprehensive chemical characterization revealed fifty constituents, including steroidal saponins, flavonoids, amino acids, organic acids, phytohormones, phenolic acids, and alkaloids. Diosgenin, Quercetin, Kaempferol, Ecdysone, and α-linolenic acid were identified as main constituents with acne-treating potential. Core targets included SRC, MAPK3, and MAPK1, with key signaling pathways implicated. Histologically, AGPP mitigated acne-induced follicular dilatation and inflammation, inhibiting inflammatory cytokine production (IL-6, IL-1ß, TNF-α). This study offers insight into AGPP's mechanism for acne treatment, laying groundwork for Paris development and drug discovery.

Qualitative and Untargeted Volatilome Fingerprinting of Aspergillus sp. and Bulbithecium sp. by HS-SPME-GCMS and Functional Interactions.

Research on fungal volatile organic compounds (VOCs) has increased worldwide in the last 10 years, but marine fungal volatilomes remain underexplored. Similarly, the hormone-signaling pathways, agronomic significance, and biocontrol potential of VOCs in plant-associated fungi make the area of research extremely promising. In the current investigation, VOCs of the isolates-Aspergillus sp. GSBT S13 and GSBT S14 from marine sediments, and Bulbithecium sp. GSBT E3 from Eucalyptus foliage were extracted using Head Space solid phase microextraction, followed by gas chromatography-mass spectrometry, identification, statistical analyses, and prediction of functions by KEGG COMPOUND and STITCH 5.0 databases. The significance of this research is fingerprinting VOCs of the isolates from distinct origins, identification of compounds using three libraries (NIST02, NIST14, and W9N11), and using bioinformatic tools to perform functional analysis. The most important findings include the identification of previously unreported compounds in fungi-1-methoxy naphthalene, diethyl phthalate, pentadecane, pristane, and nonanal; the prediction of the involvement of small molecules in the degradation of aromatic compound pathways and activation, inhibition, binding, and catalysis of metabolites with predicted protein partners. This study has ample opportunity to validate the findings and understand the mechanism or mode of action, the interspecies interactions, and the role of the metabolites in geochemical cycles.

Unravelling the metabolomic diversity of pigmented and non-pigmented traditional rice from Tamil Nadu, India.

Rice metabolomics is widely used for biomarker research in the fields of pharmacology. As a consequence, characterization of the variations of the pigmented and non-pigmented traditional rice varieties of Tamil Nadu is crucial. These varieties possess fatty acids, sugars, terpenoids, plant sterols, phenols, carotenoids and other compounds that plays a major role in achieving sustainable development goal 2 (SDG 2). Gas-chromatography coupled with mass spectrometry was used to profile complete untargeted metabolomics of Kullkar (red colour) and Milagu Samba (white colour) for the first time and a total of 168 metabolites were identified. The metabolite profiles were subjected to data mining processes, including principal component analysis (PCA), Orthogonal Partial Least Square Discrimination Analysis (OPLS-DA) and Heat map analysis. OPLS-DA identified 144 differential metabolites between the 2 rice groups, variable importance in projection (VIP) ≥ 1 and fold change (FC) ≥ 2 or FC ≤ 0.5. Volcano plot (64 down regulated, 80 up regulated) was used to illustrate the differential metabolites. OPLS-DA predictive model showed good fit (R2X = 0.687) and predictability (Q2 = 0.977). The pathway enrichment analysis revealed the presence of three distinct pathways that were enriched. These findings serve as a foundation for further investigation into the function and nutritional significance of both pigmented and non-pigmented rice grains thereby can achieve the SDG 2.

Data independent acquisition for gas chromatographic MS/MS analysis of volatile compounds.

This study presents a novel tandem mass spectrometry (MS/MS) approach utilizing a data independent acquisition (DIA) concept specifically designed with gas chromatography-electron ionization-triple quadrupole mass spectrometry (GC-EI-QqQMS). This allows compound identification based on comparison between all the experimental MS/MS product ion spectra and the simulated library data of >1,000 MS/MS transitions of 71 compounds. The simulation data were generated by using the Competitive Fragmentation Modeling (CFM-ID) 3.0 program. The approach for calculation of the DIA MS/MS library match scores was then established and applied for identification of a range of terpenoids and oxygenated compounds in perfume. The identity of each peak was confirmed using 4-241 MS/MS transitions. The established data collection and analysis methods are expected to be useful for increased confidence in volatile compound analysis.

A high-throughput analysis of volatile compounds with various polarities using headspace stir bar sorptive extraction.

Long sample extraction time is usually necessary in the analysis of volatile flavour compounds to achieve high extraction efficiency. However, the long extraction time reduces sample throughput, which results in waste of labour and energy. Therefore, in this study, an improved headspace-stir bar sorptive extraction was developed to extract volatile compounds with varying polarities in a short time. With the aim of achieving high throughput, extraction conditions were selected and optimised based on the combinations of different extraction temperatures (80-160 °C), extraction times (1-61 min), and sample volumes (50-850 µL) through the response surface methodology with Box-Behnken design. After obtaining the preliminary optimal conditions (160 °C, 25 min, and 850 µL), the effect of cold stir bars with shorter extraction time on the extraction efficiency was evaluated. The cold stir bar improved the overall extraction efficiency with better repeatability, and the extraction time was further shortened to 1 min. Then, the effects of different ethanol concentrations and salt additions (sodium chloride or sodium sulfate) were studied, and 10% ethanol concentration with no salt addition provided the highest extraction efficiency for most compounds. Finally, it was verified that the high-throughput extraction condition was feasible for the volatile compounds spiked in a honeybush infusion.

Ultra-High-Resolution Liquid Chromatography Coupled with Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry Analysis of Tessaria absinthioides (Hook. & Arn.) DC. (Asteraceae) and Antioxidant and Hypocholesterolemic Properties.

Recently, we reported the chemical profile and the hypocholesterolemic effects of a decoction of Tessaria absinthioides (Hook. & Arn.) DC. (Asteraceae). In this study, we evaluated a methanolic extract (METa) instead. Metabolite profiling was conducted using ultra-high-resolution liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC-ESI-QTOF-MS), identifying thirty compounds, including flavonoids, phenolic acids, fatty acids, and phorbolesters. Antioxidant properties were assessed through 2,2-diphenyl-1-picrylhydrazyl (DPPH), Trolox equivalent antioxidant activity (TEAC), ferric-reducing antioxidant power (FRAP), and inhibition of lipid peroxidation in erythrocytes (ILP) assays, exhibiting robust antioxidant activity. The in vivo impact of METa on serum lipid parameters and liver X receptors (LXRs) was evaluated in a hypercholesterolemic animal model. After 14 days on a high-fat diet, male rats received either a vehicle (V) or METa100, METa200 or METa500 (100; 200 and 500 mg METa/kg animal, respectively) for an additional two weeks. METa500 reduced total cholesterol levels (17.62%; p < 0.05) and all doses increased high-density lipoprotein cholesterol levels (METa100: 86.27%; METa200: 48.37%, and METa500: 29.42%; p < 0.0001). However, METa did not alter LXRs expression. The observed antioxidant and hypocholesterolemic properties of METa may be linked to the presence of six di-caffeoylquinic acids. These findings underscore T. absinthioides as a potential candidate for the treatment of metabolic disease.

Characterizing Powdered Activated Carbon Treatment of Surface Water Samples Using Polarity-Extended Non-Target Screening Analysis.

Advanced wastewater treatment such as powdered activated carbon (PAC) reduces the load of organic micropollutants entering the aquatic environment. Since mobile and persistent compounds accumulate in water cycles, treatment strategies need to be evaluated for the removal of (very) polar compounds. Thereby, non-targeted analysis gives a global picture of the molecular fingerprint (including these very polar molecules) of water samples. Target and non-target screening were conducted using polarity-extended chromatography hyphenated with mass spectrometry. Samples treated with different types and concentrations of PAC were compared to untreated samples. Molecular features were extracted from the analytical data to determine fold changes, perform a principal component analysis and for significance testing. The results suggest that a part of the polar target analytes was adsorbed but also some byproducts might be formed or desorbed from the PAC.

Effects of Lacticaseibacillus rhamnosus LOCK900 on Development of Volatile Compounds and Sensory Quality of Dry Fermented Sausages.

Traditional dry fermented meat products are highly appreciated by consumers. A probiotic starter culture increases their attractiveness through sensory qualities and a potential health-promoting effect. The ability to scale the laboratory solution to industrial conditions is an additional scientific and practical value of a new way of using probiotics in the meat industry. The aim was to evaluate the influence of the probiotic starter culture Lacticaseibacillus rhamnosus LOCK900 on the development of volatile organic compounds and the sensory quality of dry fermented pork sausages during fermentation and refrigeration storage. The microbiological and sensory characteristic (QDA method) and volatile compound (gas chromatography coupled with mass spectrometry: GC-MS) were evaluated. The number of LOCK900 cells during 12 weeks of storage remained above 6 log CFU g-1, making this product a functional food. The addition of probiotic LOCK900 increased the levels of acidic volatile compounds, aldehydes, and esters, which, combined with the additives and spices used, had a positive effect on the sensory properties of ripening sausages. The sausages with LOCK900 were characterised by positive sensory features, and their overall quality remained high during storage and did not differ from that of the control sausages.

Voltametric Determination of Zoledronic Acid in a Pharmaceutical Formulation

Objectives: The aim of this study is to study the electroactivity of zoledronic acid (ZOL), optimize the parameters affecting voltametric analysis of ZOL, and make a comparison between voltametric methods used to assay ZOL. Materials and Methods: Three voltametric methods, cyclic voltammetry (CV), square wave voltammetry (SWV), and differential pulse voltammetry (DPV), were used to determine the concentrations of ZOL solutions (0.25-1.2 mg.mL-1). Britton-Robinson universal buffer solutions (BRB) were used as supporting electrolytes with a glassy carbon working electrode. Results: The calibration plots were linear in the range from 0.20 to 1.2 mg.mL-1 for differential DPV and CV and from 0.09 to 1.2 mg.mL-1 for SWV. DPV showed the highest correlation coefficient R2 value of 0.993 and the lowest limit of detection (LOD) of 37.2 µg.mL-1. Furthermore, DPV exhibited the highest precision with the lowest relative standard deviations (RSD) values. For a commercial product of ZOL, DPV showed the best accuracy and precision with 102.32% recovery and 2.88% RSD. Conclusion: ZOL is an electroactive compound. The pH of the BRB supporting the electrolyte is important for ZOL electroactivity. DPV is the recommended method for voltametric analysis of ZOL because of its high-performance regarding accuracy, precision, and LOD compared with other studied methods.

The Application of Chemometrics to Volatile Compound Analysis for the Recognition of Specific Markers for Cultivar Differentiation of Greek Virgin Olive Oil Samples.

In the present study, volatile compound analysis of olive oil samples belonging to ten Greek cultivars was carried out. A total of 167 olive oil samples collected from two consecutive harvest years were analyzed by Head Space-Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS). Volatile compound data were combined with chemometric methods (Multivariate Analysis of Variance (MANOVA) and Linear Discriminant Analysis (LDA)) with the aim not only to differentiate olive oils but also to identify characteristic volatile compounds that would enable differentiation of botanical origin (marker compounds). The application of Stepwise LDA (SLDA) effectively reduced the large number of statistically significant volatile compounds involved in the differentiation process, and thus, led to a set of parameters, the majority of which belong to compounds that are highly dependent on variety. In addition, the use of these marker compounds resulted in an increased correct classification rate (85.6%) using the cross-validation method indicating the validity of the model developed despite the use of a large number of dependent variables (cultivars).

Simultaneous voltammetric determination of glutathione, doxorubicin and tyrosine based on the electrocatalytic effect of a nickel(II) complex and of Pt:Co nanoparticles as a conductive mediator.

Glutathione (GSH) is an important tripeptide that plays an important role in preventing damage to reactive oxygen species. An electrochemical assay was fabricated for this purpose by modification of a carbon paste electrode (CPE) with bis(1,10-phenanthroline)(1,10-phenanthroline-5,6-dione)nickel(II) hexafluorophosphate (BPPDNi) as new electro-catalyst and Pt:Co nanoparticle (Pt:CO-NPs) as highly conductive mediator. The analyses were performed at a scan rate of 10 mV/s and at a pH value of 7.4. The BPPDNi/Pt:CO-NPs/CPE showed a high sensitivity and good selectivity for electro-catalytic determination of glutathione (GSH) in nano-molar concentration range. In addition, the BPPDNi/Pt:CO-NPs/CPE was used for the determination of glutathione in the presence of doxorubicin (DOX) and tyrosine (Tyr) with three separated oxidation signals ~160 mV, ~385 mV and ~790 mV vs. Ag/AgCl/KClsat, respectively. The peak currents of the square wave voltammetric analyses were linearly dependent on glutathione, doxorubicin and tyrosine concentrations in the respective ranges of 0.001-450, 0.5-300 and 1.0-650 µM, with detection limits of 0.5 nM, 0.1 µM and 0.6 µM, respectively. Graphical abstract The first analytical sensor for simultaneous determination of glutathione, doxorubicin and tyrosine.

Effect of NaCl substitutes on lipid and protein oxidation and flavor development of Harbin dry sausage.

The effects of partially replacing NaCl with sodium substitutes (SS) on the lipid and protein oxidation and flavor development of Harbin dry sausage was investigated. There were three salt formulations, including a control (100% NaCl), NaCl partially substituted with KCl (SS1) (70% NaCl and 30% KCl), and NaCl partially substituted with KCl combined with other components (SS2) (70% NaCl, 20% KCl, 4% lysine, 1% alanine, 0.5% citric acid, 1% Ca-lactate and 3.5% maltodextrin). The levels of lipid and protein oxidation increased in all sausages during fermentation (P < 0.05). In addition, lower oxidation of lipids and proteins were found in the SS2 treatment (P < 0.05) due to the lower NaCl concentration. The SS, especially the SS2, promoted the formation of volatile compounds originated from carbohydrate and amino acid metabolism, ß-lipid oxidation and esterification; however, this substitute inhibited the formation of volatile compounds originated from lipid autooxidation (P < 0.05). Overall, SS2 could improve the flavor development of Harbin dry sausage and reduce NaCl by 30%.

Matrix-free laser desorption ionization mass spectrometry as a functional tool for the analysis and differentiation of complex phenolic mixtures in propolis: a new approach to quality control.

Matrix-free laser desorption ionization (LDI) is a rapid and versatile technique for the ionization of small, UV-light-absorbing molecules. Indeed, many natural products such as polyphenols exhibit inherent LDI properties, potentially facilitating their detection from highly complex samples such as crude extracts. With this in mind, the present work thoroughly evaluated the potential of LDI as an analytical tool for the chemical profiling and differentiation of propolis samples obtained from different global regions. Propolis is a complex bee product containing, among others, significant amounts of phenolic constituents that may show LDI effects. The present work will demonstrate that LDI not only provides reproducible and highly specific fingerprint spectra for each of the tested samples, it further allows their clear differentiation by principal compound analysis (PCA). Contrary to classical analytical approaches such as LC- or GC-MS, LDI does not require time-consuming sample preparation and method optimization procedures. Thus, the technique represents a most interesting analytical tool and potent supplement to classic LC-MS for quality control of herbal pharmaceuticals and dietary supplements. Present results clearly support this approach and further suggest the use of LDI as a versatile tool for the automated analysis of large sample batches on an industrial scale. Graphical abstract ᅟ.

Classifying Degraded Modern Polymeric Museum Artefacts by Their Smell.

The use of VOC analysis to diagnose degradation in modern polymeric museum artefacts is reported. Volatile organic compound (VOC) analysis is a successful method for diagnosing medical conditions but to date has found little application in museums. Modern polymers are increasingly found in museum collections but pose serious conservation difficulties owing to unstable and widely varying formulations. Solid-phase microextraction gas chromatography/mass spectrometry and linear discriminant analysis were used to classify samples according to the length of time they had been artificially degraded. Accuracies in classification of 50-83 % were obtained after validation with separate test sets. The method was applied to three artefacts from collections at Tate to detect evidence of degradation. This approach could be used for any material in heritage collections and more widely in the field of polymer degradation.

Matrix-assisted laser desorption/ionization mass spectrometry for the analysis of polyamines in plant micro-tissues using cucurbituril as a host molecule.

In this study, a matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) strategy using cucurbit[n]uril (CB[n]) as a host molecule is proposed for the analysis of low molecular weight (LMW) compounds in complex samples. As a proof-of-concept, CB[6] was selected as the host molecule, and endogenous polyamines in plant tissue were chosen as the target analytes. Due to the molecular recognition and mass shifting properties of CB[6], the ionic signals associated with polyamines were moved to the higher mass region (>1000 Da) after specifically binding to CB[6], while signal interference derived from the conventional organic matrix and the complex sample matrix remained in the low mass region because of the incompatibility of their molecular size with CB[6] cavities. The strategy not only facilitated the analysis of LMW compounds in complex samples by MALDI MS, but also offered high throughput by accomplishing the entire analytical procedure within 10 min. The detection of polyamine concentration showed good linearity in the range of 0.02-10.0 ng/µL with correlation coefficients (R) greater than 0.9915. The limits of detection were 8.8-28.8 pg. The good reproducibility and reliability of the method were demonstrated by excellent intraday and interday precisions with relative standard deviations less than 7.9%, and the recovery ranged from 92.1% to 117.1%. Finally, the good sensitivity of the method allowed for the quantitative analysis of endogenous polyamine concentrations in various micro-tissues of Arabidopsis thaliana (20.0-740.0 µg fresh weight for each sample).

The contribution of aromatic components in Katsuobushi to preference formation and reinforcement effect.

Katsuodashi, a dried bonito broth, is very basic and indispensable in Japanese cuisine and contains taste-exhibiting components and unique aroma. We previously reported that its unique aroma contributes to the preference and reinforcement effect associated with dried bonito. This study aims to elucidate the contribution of aromatic components in Katsuobushi to preference formation and reinforcement effect. Volatile components obtained from dried bonito were fractionated and the fractions were subjected to two-bottle choice test. The fractionation test suggested that the component responsible for the preference is not one but comprises multiple components. In the GC-MS analysis/reconstruction test, solution with aromatic flavor narrowed down to 125 compounds had preference, and also had reinforcement effect. Moreover, GC-MS-olfactometry analysis narrowed down the candidate components to 28 out of 125. Mice showed preference for the test solution with aromatic flavor reconstructed with 28 components but did not show reinforcement behavior.

Characterization of drug authenticity using thin-layer chromatography imaging with a mobile phone.

Thin-layer chromatography (TLC) has a myriad of separation applications in chemistry, biology, and pharmacology due to its simplicity and low cost. While benchtop laboratory sample application and detection systems for TLC provide accurate quantitation of TLC spot positions and densities, there are many applications where inexpensive and portable instruments would greatly expand the applicability of the technology. In this work, we demonstrate identity verification and concentration determination of pharmaceutical compounds via TLC using a custom 3D-printed cradle that interfaces with an ordinary mobile phone. The cradle holds the mobile phone's internal, rear-facing camera in a fixed position relative to a UV lamp and a TLC plate that includes a phosphor in the stationary phase. Analysis of photographs thus reveals the locations and intensities of principal spots of UV--absorbing drugs. Automated image analysis software determines the center location and density of dark spots, which, using integrated calibration spots of known drug compounds and concentrations, can be used to determine if a drug has been diluted or substituted. Two independent image processing approaches have been developed that may be selected based upon the processing capabilities of the smartphone. Each approach is able to discern 5% drug concentration differences. Using single-component solutions of nevirapine, amodiaquine, and paracetamol that have been manually applied, the mobile phone-based detection instrument provides measurements that are equivalent to those obtained with a commercially available lab-based desktop TLC densitometer.

Evaluation of baker's yeast strains exhibiting significant growth on Japanese beet molasses and compound analysis of the molasses types.

Cane molasses, most of which is imported, is used as a raw material for production of baker's yeast (Saccharomyces cerevisiae) in Japan. On the other hand, beet molasses is scarcely used for this purpose, but it can be of great advantage to cane molasses because it is domestically produced in relatively high amounts as a by-product of beet sugar processing. However, the yield of baker's yeast is sometimes low with Japanese beet molasses compared to imported cane molasses. For the production of baker's yeast with Japanese beet molasses, we evaluated S. cerevisiae strains, including industrial and laboratory strains, to group them according to the growth profile on beet and cane molasses. To discuss the factors affecting growth, we further analyzed the major compounds in both types of molasses. Beet molasses seems to contain compounds that promote the growth of beet molasses-favoring strains rather than inhibit the growth of cane molasses-favoring strains. It was assumed that α-amino acid was one of the growth promotion factors for beet molasses-favoring strains.

Separation of 1,3-dimethylamylamine and other polar compounds in a dietary supplement formulation using aqueous normal phase chromatography with MS.

Five ingredients (caffeine, L-arginine, creatine, ß-alanine, and 1,3-dimethylamylamine) from a workout supplement were separated by HPLC with UV detection and LC-MS using an analytical column based on silica hydride operating in aqueous normal phase mode. While RP methods were observed to be inadequate for the analysis due to low retention, aqueous normal phase chromatography was able to readily retain and resolve the analytes. After method development on the HPLC-UV system, the conditions were successfully transferred to an LC-MS system for analysis. Based on calibration curve data, estimates of 63.5, 380.3, and 13.1 mg/serving (5.50 g) were obtained for creatine, l-arginine, and 1,3-dimethylamylamine, respectively. Standard addition data results were compared to those of the calibration curve study, and the two values differed by less than 1% in the case of creatine. The conditions are suitable for further development as a reliable means of quantitating the analytes in workout supplement formulations.