Search Results (143)

The changes in monovarietal extra virgin olive oils (EVOOs), produced with olives grown under different agronomic conditions, were investigated by targeted and untargeted analytical approaches. Specifically, volatile molecules were monitored in oils just produced and stored for 6 and 12 months with two different packaging solutions. The targeted SPME-GC–MS method showed an increase in volatile markers of lipid oxidation. Moreover, more rapid analytical approaches, namely targeted HS-GC–IMS and untargeted FGC, were used to investigate volatile organic compounds (VOCs). These chromatographic methods, respectively, returned heatmaps and fingerprint profiles that were elaborated on by multivariate analysis. Exploratory principal component analysis performed on the data from VOCs allowed the clustering of samples based on the storage time. The quality of samples was also determined by a panel test. Furthermore, this study employed previously built models using partial least squares discriminant analysis to confirm the sensory classification of the stored samples. Based on these predictive models, all samples were confirmed as EVOO, except for one categorized as virgin (rancid according to the panel test). This classification was further supported by the SPME-GC–MS analysis, which revealed higher concentrations of lipid oxidation markers in this specific sample, in particular the (E)-2-heptenal reached a concentration twenty times higher than its odor threshold. In addition, five oils were inconsistently classified by the models and considered at risk of downgrading the commercial category after 12 months of storage. Full article

Zanthoxylum bungeanum Maxim. (huajiao) and Zanthoxylum armatum DC. (tengjiao), also known as Sichuan pepper, is a popular spice owing to its unique aroma and taste. Fried pepper oils are liquid condiments with unique flavors extracted from the pericarps of huajiao and tengjiao. To investigate the volatile profiles of the two different fried pepper oils, solid-phase microextraction (SPME) coupled with gas chromatography–mass spectrometry (GC-MS) was employed. The results revealed that D-limonene, linalyl acetate, linalool, myrcene, and ocimene significantly contributed to the overall flavor of huajiao oils. In addition, linalool, D-limonene, sabinene, myrcene, and linalyl acetate were identified as the main odorants in tengjiao oils. Finally, a characteristic chromatogram for the volatile compounds of each oil was established through the Similarity Evaluation System for the Chromatographic Fingerprint of Traditional Chinese Medicine, and the similarity thresholds of huajiao oils and tengjiao oils were 0.984 and 0.998, respectively. Linalool, sabinene, and linalyl acetate were markers for distinguishing between ZAOV samples and ZAOC samples. And germacrene D, linalool, sabinene, linalyl acetate, and β-myrcene were markers for distinguishing ZBOV samples from ZBOC samples. Full article

Polygonatum sibiricum (P. sibiricum) is a significantly health-promoting plant unique in medicine and food. Currently, research on the bioactive components of P. sibiricum primarily focuses on polysaccharides. According to the Chinese Pharmacopoeia, the polysaccharide content in P. sibiricum must be at least 7.0%, which is the only criterion used for determining its content. In contrast, this study aims to thoroughly investigate and clarify the various components that contribute to the therapeutic and functional properties of P. sibiricum. We seek to broaden the focus beyond polysaccharides to identify other potentially significant bioactive substances. We established High-Performance Liquid Chromatograph (HPLC) fingerprints for wine-processed P. sibiricum from various regions and identified 17 common peaks. The antioxidant activities of these components were assessed using ABTS and DPPH methods. The spectrum–effect relationship was elucidated through partial least squares regression and grey relational analysis. The results revealed that the antioxidant active components in wine-processed P. sibiricum include 5-hydroxymethylfurfural, p-hydroxycinnamic acid, myricetin, caffeic acid, vanillic acid, and adenosine. This research not only clarifies the antioxidant material basis of wine-processed P. sibiricum but also establishes a scientific foundation for enhanced quality control in future applications. Full article

The dynamic development of various branches of medicine and pharmacy, along with the emergence of new preventive and alternative therapies for various diseases, creates opportunities for new solutions utilizing carriers of active substances. Their therapeutic effect may occur through direct contact with skin lesions or indirectly, where medicinal substances penetrate the capillary network in the deeper layers of the skin and reach the bloodstream. The aim of the research was to obtain carriers with a matrix consisting of two renewable-source polymers (chitosan and ethylcellulose) and a core material derived from Ginkgo biloba green leaf extract (GBE). The obtained ethylcellulose microcapsules with encapsulated chitosan nanoparticles with extract {Et[Ch(GB)NP]} were characterized with respect to size, shape, surface morphology (SEM microscopy), and active substance release kinetics (UV-VIS and mathematical release models). The kinetics of active substance release were analyzed using UV-VIS spectroscopy and mathematical release models. The released active components were assessed microbiologically for activity against six bacterial strains and two fungal strains, as well as chromatographically using HPLC-ESI-QTOF-MS/MS fingerprinting. The microcapsules with a dual polymer layer exhibited a slow release of the core material, which demonstrated microbiological activity. The strongest antimicrobial effects were observed against Klebsiella pneumoniae and Salmonella enteritidis, with a minimum inhibitory concentration (MIC) of 410 µg/mL. The release of the core material from the double-layer polymer structures was more efficient in a physiological saline environment, with the best fit for the extract release kinetics following a zero-order model (regression coefficient R² = 0.9939). The obtained microcapsules with a dual polymer layer show great potential for therapeutic applications in the medical industry. Their controlled release properties and antibacterial effectiveness make them a promising carrier for active substances in modern therapies. Full article

Chromatographic fingerprint technology has become the standard of quality control for traditional herbal medicines (THMs). But several issues are associated with the wavelength selection of the representative fingerprint, such as contradictory evaluation results at different wavelengths and the accurate quantification of each composition at one wavelength. These problems can be addressed by projection profiling. Projection profiling is a collection of all sample compositions at the maximum absorption wavelength after baseline correction. In this paper, eleven baseline correction algorithms are optimized by using the effective information factor (EI) as an indicator. The influence of different integration methods and wavelengths on analytical method validation and similarity analysis results are discussed in detail to clarify the advantages of the projection profiling. A total of 33 batches of Compound Licorice Tablets (CLTs) were used to show the influence of different wavelengths in a similarity evaluation. The results show that projection profiling is a better choice than any chromatogram at a certain wavelength, because projection profiling is more informative, accurate, and stable. Full article

The mangrove ecosystem is reported to have a large diversity of species that develop in environments with high salinity levels. Plant species from mangroves are used in traditional medicine and are potential sources of chemicals entities with therapeutic applications. The present work aims to assess and document the influence of salinity on the antioxidant activity exerted by extracts of mangrove species through spectroscopic and chemical analysis. The highest salinity is recorded in Río Verde (RV) in Petén Neyac (PN), an LPBR site. The leaves of Laguncularia racemosa (from RV and PN) recorded the highest extraction yield (35.29 ± 0.45%). Phytochemical analysis indicated the presence of several families of secondary metabolites in the leaves of Rhizophora mangle, Avicennia germinans, and L. racemosa collected in PN and RV, and the chromatographic profile confirms the complexity of the extracts, especially in L. racemosa-RV. The highest content of chlorophylls, carotenoids, and simple phenols was recorded in R. mangle (in RV and PN); flavonoids were high in A. germinans (RV), and the highest antioxidant activity was recorded in L. racemosa (RV) using the DPPH model (EC₅₀: 39.74 ± 0.91 μg/mL; E_max: 67.82 ± 1.00%). According to HPLC, gallic acid (GA), and quercetin (Q) are important metabolites in L. racemosa. FTIR spectra can identify several chemical groups and fingerprint regions in complex mixtures, such as methanolic extracts of the species under study. In this context, this is the first report on chemical changes resulting from species collected at sites with different degrees of salinity. GA is the main metabolite affected by salinity and participates in the antioxidant activity exerted by the original extract, which could explain the physiological adaptations of L. racemosa and its traditional uses. L. racemosa (RV) is ideal for a bioguided phytochemical study that would yield valuable knowledge about its medicinal properties, support ecological conservation, and drive innovation across multiple industries. Further analytical studies are needed to corroborate the impact of salinity on the biosynthesis of secondary metabolites. Full article

This study aimed to characterize the metabolomic profile of monofloral honey from Eucryphia cordifolia (ulmo) and evaluate the potential transfer of bioactive compounds from the plant parts, including the leaves and flowers, to the honey. Using UHPLC/Q-TOF-MS analysis, various flavonoids and phenolic acids were identified and quantified in extracts from the leaves, flowers, and honey from E. cordifolia. Given their rich polyphenolic composition, E. cordifolia leaves were included in this study to assess their potential contribution to the antioxidant properties and chemical markers of ulmo honey. Additionally, the polyphenolic compounds in honey samples were quantified. Chromatographic analysis via UHPLC-MS/MS revealed that ulmo honey contains phenolic acids such as gallic, syringic, ferulic, chlorogenic, caffeic, and coumaric acid, as well as flavonoids including pinocembrin, quercetin, luteolin, kaempferol, epicatechin, apigenin, and isorhamnetin. The results indicate that pinocembrin and gallic acid are the main chemical markers of ulmo honey, while isorhamnetin could complement its characterization as a complementary marker. UHPLC/Q-TOF-MS analysis was also utilized to compare the compounds present in the honey with those found in the plant parts (leaves and flowers), respectively. A total of 10 shared compounds were identified, 9 of which were preliminarily identified, while 1 remains unknown. Notably, dihydroquercetin 3-O-rhamnoside, quercetin 3-O-rhamnoside, cyanidin 3-(p-coumaroyl)-glucoside, and eupatorin were detected in ulmo honey for the first time. Along with gallic acid, pinocembrin, and isorhamnetin, these compounds could contribute to a characteristic fingerprint for identifying the botanical origin of the honey. Overall, these findings provide valuable insights into the chemical composition of ulmo honey and its potential application as a functional product with antioxidant properties. Full article

This study reports for the first time the fingerprinting extractives analysis of the indigenous wood species of Podocarpus totara from New Zealand, Eucalyptus saligna from Australia and Pinus radiata imported from California, USA and grown in New Zealand. We evaluated the use of analytical techniques for wood species discrimination. We compared the chemical fingerprinting of extractive compounds obtained using traditional chromatographic techniques with direct analysis in real-time–time of flight-mass spectrometry (DART-TOF-MS) with the auxiliary of chemometrics and principal component analysis. The traditional wet chemistry analysis of wood extracts provided a comprehensive characterisation of all extractive components. However, the more eco-friendly, sustainable and faster DART-TOF-MS technique effectively distinguished between wood species when heartwood and sapwood samples were combined. Notably, neither wet chemistry nor DART-TOF-MS could clearly differentiate between heartwood and sapwood within the same wood species. DART-TOF-MS analysis demonstrates potential as a reliable quality control tool for identifying wood species necessary in commercial and timber trading markets as well as for detecting the illicit trade of counterfeit wood products. Full article

Background and Objectives: As a medicinal and food homologous substance, Eupolyphaga steleophaga is renowned for its potential health benefits, including anti-tumor effects, immune system support, and anti-inflammatory properties. Eupolyphaga steleophaga polypeptides have demonstrated significant biological activity, including the regulation of coagulation and lipid metabolism. However, the peptide composition of Eupolyphaga steleophaga requires further clarification to facilitate quality control improvements and a deeper investigation into its pharmacological effects. Therefore, this study aimed to simulate the digestive absorption process of Eupolyphaga steleophaga following oral administration and identify its enzymatic components to enhance quality control. Methods: The digestive absorption process was simulated using artificial gastric fluid and pepsin. A fingerprinting method based on ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC-MS)(Acquire UPLC-Synapt G2-Si HDMS, Waters Corporation, Milford, MA, USA) was developed to identify 63 enzymatic components. The enzymolysis polypeptide fingerprint detection method was used to analyze 10 batches of Eupolyphaga steleophaga sourced from Harbin No. 4 Traditional Chinese Medicine Factory. Chromatographic collection was performed using an ACQUITY UPLC BHE C18 column. Gradient elution was carried out using a mixture of 0.1% formic acid with acetonitrile and 0.1% formic acid with water, with an average flow rate of 0.3 mL/min, a column temperature of 40 °C, and an injection volume of 2 μL. The mass spectrometry (MS) conditions were set as follows: the ion source was operated in positive electrospray ionization (ESI+) mode, with a capillary voltage of 2.8 kV and a sampling cone voltage of 40 V. The ion-source temperature was maintained at 110 °C, while the desolvation temperature was set to 400 °C. The cone gas flow rate was 50 L/h, and the desolvation gas flow rate was 800 L/h. The range for the collection of mass-to-charge ratios (m/z) was between 50 and 1200. Results: The UHPLC-MS method demonstrated high accuracy, repeatability, and stability, successfully identifying 63 enzymatic components of Eupolyphaga steleophaga. Furthermore, polypeptide markers for 63 selected components were identified in all 10 batches of Eupolyphaga steleophaga medicinal materials. This approach was validated by including numerical values such as retention times and peak areas, confirming its reliability for quality control enhancement. Conclusions: This novel UHPLC-MS approach serves as a powerful tool for advancing quality control strategies in veterinary medicine, particularly for animal-derived medicines. It lays a solid foundation for subsequent pharmacological studies of Eupolyphaga steleophaga polypeptides, offering a more reliable means to explore their biological activities and therapeutic potential. Full article

In this study, hybrid materials were synthesized incorporating curcumin, Cu²⁺ or Fe³⁺, and Kappa-carrageenan as a reducing agent to improve stability, considering that curcumin has low thermal and solution stability, which limits its applications. Colorimetric analysis showed color changes in the hybrids, ultraviolet–visible spectroscopy revealed band shifts in the hybrids, and infrared analysis indicated shifts in wavenumbers, suggesting changes in the vibrational state of curcumin after bonding with metal ions. These techniques confirmed the formation of hybrid materials. Thermogravimetric and chromatographic analyses demonstrated greater thermal and solution stability for the hybrids compared to curcumin. Additionally, the hybrid composites effectively developed natural and sebaceous latent fingerprints with good clarity and contrast on glass surfaces. Both composites performed similarly to commercial Gold^® powder. When applied to surfaces representative of forensic scenarios, the composites were versatile, revealing sufficient fingerprint details for human identification on both porous and non-porous surfaces. Scanning electron microscopy images showed greater clarity in sebaceous and natural fingerprints developed with the Fe composite compared to the Cu composite. Full article

Raman spectroscopy is a technique which involves quantitative and qualitative molecular analysis based on the interaction between incident light and isolation of scattered wavelengths in generating a molecular fingerprint. It has a broad array of potential scientific applications, encompassing areas as diverse as food science and forensics. However, it may also be highly useful in clinical oncology. A recent focus of research in oncology has been in achieving the individualisation of care. Two important strategies to achieve a so-called “precision oncology” approach may include the detection of circulating tumour DNA (ctDNA) in more objectively evaluating treatment response and guiding de-escalation and intensification approaches in systemic therapy and therapeutic drug monitoring (TDM). Therapeutic drug monitoring involves the quantitation of plasma drug levels in order to tailor medication dosing in optimizing outcomes. The existing approaches to characterize small molecules, such as fluorescence-based and chromatographic strategies, may be limited by high costs, long turnaround times, and bulky equipment. Surface-enhanced Raman spectroscopy (SERS) may be deployed by utilizing a handheld device, with the potential for point of care, rapid turnaround, low-cost assessment of clinically relevant parameters, and prompt implementation of attendant changes in treatment. Although there is a growing body of data supporting the implementation of TDM and evaluation of ctDNA in achieving precision medicine, the uptake of such approaches remains relatively limited outside of clinical trials. As stated, the nature of existing analytical methodologies may prove to be a significant barrier to the routine clinic-based implementation of such approaches. Therefore, we provide the existing evidence for SERS in alleviating these barriers. We also provide insights into how SERS could contribute to clinical oncology. Full article

The essential oil components of traditional Chinese medicine in-hospital preparation were complex, and one-dimensional chromatographic separation was difficult to completely separate them due to the limited peak capacity. This study was carried out to establish a comprehensive two-dimensional chromatographic separation and analysis method based on countercurrent chromatography (CCC) and gas chromatography (GC). In this paper, we focused on the separation of the essential oil of the traditional Chinese medicine in-hospital preparation Wenjing Tongluo San by CCC × GC, and explored the orthogonality between the two chromatographic techniques to provide the new technical support for the screening of the active ingredients. A solvent system composed of n-hexane-ethyl acetate-methanol-water (9.5:0.5:8.5:1.5, v/v) was chosen for the first-dimensional CCC separation. All the fractions collected from CCC were transferred to GC for plotting two-dimensional contours map. The calculated capacity of the two-dimensional separation system exceeded 3000, which was 8 times more than that of the one-dimensional separation system. High orthogonality (r = 0.42) and spatial coverage factor (70.42%) were obtained. Meanwhile, all the fractions were identified by GC-MS. Our research provided a new methodology for separating essential oils in traditional Chinese medicine as well as an approach for evaluating the quality of traditional Chinese medicinal in-hospital preparation based on two-dimensional chromatographic fingerprints. Full article

In food authentication, it is important to compare different analytical procedures and select the best method. The aim of this study was to determine the fingerprints of Zweigelt and Rondo wines through headspace analysis using ultra-fast gas chromatography (ultra-fast GC) and to compare the effectiveness of this approach at classifying wines based on grape variety and type of malolactic fermentation (MLF) as well as its greenness and practicality with three other chromatographic methods such as headspace solid-phase microextraction/gas chromatography-mass spectrometry with carboxen-polydimethylosiloxane fiber (SPME/GC-MS with CAR/PDMS fiber), headspace solid-phase microextraction/gas chromatography-mass spectrometry with polyacrylate fiber (SPME/GC-MS with PA fiber), and ultra performance liquid chromatography–photodiode array detector-tandem mass spectrometry (UPLC-PDA-MS/MS). Principal Component Analysis (PCA) revealed that fingerprints obtained using all four chromatographic methods were suitable for classification using machine learning (ML). Random Forest (RF) and Support Vector Machines (SVM) yielded accuracies of at least 99% in the varietal classification of Zweigelt and Rondo wines and therefore proved suitable for robust fingerprinting-based Quality Assurance/Quality Control (QA/QC) procedures. In the case of wine classification by the type of MLF, the classifiers performed slightly worse, with the poorest accuracy of 91% for SVM and SPME/GC-MS with CAR/PDMS fiber, and no less than 93% for the other methods. Ultra-fast GC is the greenest and UPLC-PDA-MS/MS is the most practical of the four chromatographic methods. Full article

As a part of the important species that form coral reef ecosystems, stony corals have become a potential source of pharmacologically active lead compounds for an increasing number of compounds with novel chemical structures and strong biological activity. In this study, the secondary metabolites and biological activities are reported for Aspergillus terreus C21-1, an epiphytic fungus acquired from Porites pukoensis collected from Xuwen Coral Reef Nature Reserve, China. This strain was cultured in potato dextrose broth (PDB) media and rice media with different salinities based on the OSMAC strategy. The mycelial morphology and high-performance thin layer chromatographic (HPTLC) fingerprints of the fermentation extracts together with bioautography were recorded. Furthermore, an untargeted metabolomics study was performed using principal component analysis (PCA), orthogonal projection to latent structure discriminant analysis (O-PLSDA), and feature-based molecular networking (FBMN) to analyze their secondary metabolite variations. The comprehensive results revealed that the metabolite expression in A. terreus C21-1 differed significantly between liquid and solid media. The metabolites produced in liquid medium were more diverse but less numerous compared to those in solid medium. Meanwhile, the mycelial morphology underwent significant changes with increasing salinity under PDB cultivation conditions, especially in PDB with 10% salinity. Untargeted metabolomics revealed significant differences between PDB with 10% salinity and other media, as well as between liquid and solid media. FBMN analysis indicated that alkaloids, which might be produced under high salt stress, contributed largely to the differences. The biological activities results showed that six groups of crude extracts exhibited acetylcholinesterase (AChE) inhibitory activities, along with 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging and antibacterial activities. The results of this study showed that the increase in salinity favored the production of unique alkaloid compounds by A. terreus C21-1. 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