HPLC-MS Analysis Research Articles

Chemical Characterization and Antifungal Activity of Blue Tansy (Tanacetum annuum) Essential Oil and Crude Extracts against Fusarium oxysporum f. sp. albedinis, an Agent Causing Bayoud Disease of Date Palm.

Tanacetum annuum L. is a Mediterranean plant, commonly known as Blue Tansy due to its blue colour as an essential oil, which is widely used for medicinal purposes. However, there are no studies on the bioactive compounds (especially, phenolic compounds) and the biological properties of their organic extracts. Herein, the purpose of the present work was to investigate the chemical composition of the essential oil and crude extracts of the T. annuum aerial parts collected from northern Morocco and to evaluate their antioxidant and antifungal activity against Fusarium oxysporum f. sp. albedinis, an agent causing Bayoud disease of the date palm, an important food source and commercial perennial crop in the Sahara and North Africa. Chemically, Folin-Ciocalteu and aluminium chloride colourimetric methods were used to determine the total phenolic (TPC) and total flavonoid (TFC) contents, respectively; polyphenols were characterized using HPLC-MS, while GC-MS was used to analyse the essential oil composition. Moreover, the evaluation of antioxidant and antifungal activities was carried out using the DPPH test and microdilution method, respectively. The results showed that the three T. annuum parts (stems, leaves and flowers) extracts contained important TPC and TFC with values varied between 51.32 and 116.32 mg/g of dry crude extract (DCE). HPLC-MS analysis revealed the identification and quantification of 19 phenolic acids and flavonoids with an emphasis on apigenin 7-glucoside (4540 µg/g of dry weight (DW)), luteolin 7-glucoside (2804 µg/g DW) and salicylic acid (1878 µg/g DW). Additionally, 39 biomolecules were identified in the essential oil using GC-MS, which were predominated by camphor (16.69%), α-pinene (12.37%), bornyl acetate (11.97%) and limonene (11.10%). The methanolic and hydro-methanolic extracts of T. annuum parts demonstrated a strong antioxidant property with IC50 values ranging between 0.22 and 0.65 mg/mL. Concerning antifungal activity, the essential oil and crude extracts of the Moroccan Blue Tansy exhibited a potent capacity against F. oxysporum f. sp. albedinis at low concentrations, with MIC and MFC values of 3.33 and 4.58 µL/mL for the essential oil and values of 3.33 and 9.17 mg/mL for crude extracts, respectively. Overall, these results demonstrated T. annuum as an important source of bioactive compounds and contribute significantly to the potential of using essential oils and extracts for controlling the Bayoud disease of date palms. Moreover, the finding suggests that T. annuum can be highly useful for phytosanitary and pharmaceutical industries.

Investigating the impact of pedoclimatic conditions on the oenological performance of two red cultivars grown throughout southern Italy.

The cultivated grapevine, Vitis vinifera subsp. vinifera, possesses a rich biodiversity with numerous varieties. Each variety adapts differently to varying pedoclimatic conditions, which greatly influence the terroir expression of wine regions. These conditions impact vine growth, physiology, and berry composition, ultimately shaping the unique characteristics and typicity of the wines produced. Nowadays, the potential of the different adaptation capacities of grape varieties has not yet been thoroughly investigated. We addressed this issue by studying two grape varieties, Aglianico and Cabernet Sauvignon, in two different pedoclimatic conditions of Southern Italy. We evaluated and compared the effect of different pedoclimatic conditions on plant physiology, the microbial quality of grapes using Next-Generation Sequencing (NGS) technology, the expression trends of key genes in ripe berries and the concentration of phenolic compounds in grapes and wines by HPLC-MS, HPLC-DAD, NMR and spectrophotometric analyses. Metabolomic and microbiome data were integrated with quantitative gene expression analyses to examine varietal differences and plasticity of genes involved in important oenological pathways. The data collected showed that the phenotypic response of studied grapes in terms of vigor, production, and fruit quality is strongly influenced by the pedoclimatic conditions and, in particular, by soil physical properties. Furthermore, Aglianico grape variety was more influenced than the Cabernet Sauvignon by environmental conditions. In conclusion, the obtained findings not only reinforce the terroir concept and our comprehension of grape's ability to adapt to climate variations but can also have implications for the future usage of grape genetic resources.

Extraction of Bioactive Compounds via Solid-State Fermentation Using Aspergillus niger GH1 and Saccharomyces cerevisiae from Pomegranate Peel

This study investigated the recovery of polyphenolic compounds such as punicalagin, punicalin, and ellagic acid via solid-state fermentation (SSF)-assisted extraction from pomegranate peel (Punica granatum L.) using Aspergillus niger GH1 and Saccharomhyces cerevisiae. Food processing has contributed to the increase in agroindustrial wastes, which has become a global concern due to environmental protection. However, these wastes can be valorized via the extraction of high-value components such as bioactive compounds. Ellagitannins extracted during the bioprocesses were identified via the HPLC–MS technique and quantified via total polyphenols (hydrolyzable and condensed assays). Enzymatic activities were tested. HPLC–MS analysis showed a decrease in the levels of punicalagin, the formation of punicaline, and the accumulation of ellagic acid during fermentation kinetics. The present study compares two different bioprocesses in order to obtain, from agroindustrial wastes, high-added-value compounds using SSF-.

Accelerated electron and mass transfer through constructing H2WO4/Ti3C2/g-C3N4 Z-scheme photocatalyst for environmental remediation

The catalytic efficiency of photocatalysts highly depends on electron transport and mass transfer. Herein, we designed and prepared an effective H2WO4/Ti3C2/g-C3N4 (HTC) Z-scheme heterojunction through interfacial engineering strategy. The results manifested that 97.4% of Cr(VI) (80 μM, 50 mL) could be removed by HTC heterojunction within 10 min under visible light irradiation. The reduction rate constant of Cr(VI) for H2WO4/g-C3N4 (HC) heterojunction increased by a factor of 21 after introducing the conductive Ti3C2. Moreover, 96% of tetracycline (TC, 10 mg L−1, 50 mL) could be degraded by HTC heterojunction within 30 min. The electronic conductivity and ionic diffusion coefficient of HC heterojunction increased by a factor of 64 and 1064 after adding Ti3C2, respectively. This result indicated that the introduction of highly conductive Ti3C2 significantly improved the electron and mass transfer of the heterojunction. Meanwhile, the HCT heterojunction displayed favorable photocurrent, and keep excellent photostability during the long-term test. Moreover, density functional theory (DFT) calculations demonstrated that the internal electric field (IEF) from g-C3N4 to H2WO4 in HCT heterojunction promotes the combination of the photoinduced electrons in the H2WO4 conduction band (CB) with photoinduced holes in the g-C3N4 valence band (VB), thus accelerating the charge transfer in the HCT Z-scheme heterojunction. The antibacterial efficiency of HTC heterojunction against E. coli and S. aureus could reach up to 98.4% and 99.7%, respectively. The degradation intermediates and the potential degradation mechanism of TC were analyzed and proposed based on the results of HPLC-MS analysis. Moreover, the toxicity of TC and degradation intermediates were estimated by Toxicity Estimation Software (T.E.S.T.) based on quantitative structure-activity relationship (QSAR). This work provided a valuable guideline for designing the effective MXene-based Z-scheme heterojunction for environmental remediation.

Synthesis of novel direct Z-scheme heterojunction photocatalyst from WO3 nanoplates and SrTiO3 nanoparticles with abundant oxygen vacancies

Excessive use of insecticides in agriculture has raised a global concern owing to their environmental pollution. Various techniques are utilized for removal these compounds which one of the most efficient methods is photocatalytic degradation by heterojunction nanocomposites. Herein, a direct Z-scheme heterojunction nanocomposite with abundant oxygen vacancy defects was fabricated via simple hydrothermal treatment of WO3 nanoplate and SrTiO3 nanoparticle and was utilized as a powerful photocatalyst for decomposition of nitenpyram insecticide under illumination of simulated sunlight. The findings revealed that, the heterojunction nanocomposite with 30wt% of SrTiO3 has the best photocatalytic efficiency. Improvement of the photocatalytic ability may be ascribed to the existence of oxygen vacancy defects in heterojunction interfaces between two semiconductors, facilitating of charge carriers separation, and effective generation of the •O2− and •OH radicals. Furthermore, from the results of the radical capture studies, ESR techniques, and Mott-Schottky analyses, it can be concluded that the hydroxyl radical is the major oxidant for degradation of nitenpyram, and by modulating the charge carrier dynamics and regulation of the charge transfer pathways, a direct Z-scheme heterojunction nanocomposite is formed with improved photocatalytic efficiency. Additionally, the possible decomposition intermediates of nitenpyram were detected from the HPLC-MS analysis.

Biological Activity and Metabolomics of Griffonia simplicifolia Seeds Extracted with Different Methodologies.

Griffonia simplicifolia, a tropical plant endemic to West Africa, is highly regarded for its significant pharmacological potential. The objective of this study was to evaluate the metabolomic profile and to explore the antioxidant properties, antiproliferative activity, and antimicrobial potential of G. simplicifolia seed extracts obtained through either maceration, microwave-assisted extraction (MAE), or Soxhlet extraction using water, acetone, methanol and ethanol as solvents. Overall, methanol possessed superior total extraction efficiency. HPLC analyses confirmed the efficacy of acetone and ethanol as optimal solvents for the extraction of flavonoids and flavan-3-ols, whereas MAE exhibited enhanced effectiveness in extracting N-containing compounds, including 5-hydroxytryptophan (5-HTP). HPLC-MS analyses identified forty-three compounds, including thirty-four phenolic compounds and nine N-containing molecules. Isomyricitrin, taxifolin and a flavonol glucuronide were the main polyphenols, whereas 5-HTP was the main N-containing compound. Hydroalcoholic G. simplicifolia extracts showed the highest radical scavenging and metal-reducing antioxidant power, suggesting that most of the contribution to antioxidant activity depends on the more polar bioactive compounds. G. simplicifolia extracts showed dose-dependent antiproliferative activity against three distinct cancer cell lines (HeLa, HepG2, and MCF-7), with notable variations observed among both the different extracts and cell lines and divergent GI50 values, emphasizing substantial discrepancies in cell sensitivity to the various extracts. Furthermore, G. simplicifolia extracts revealed antibiotic activity against Staphylococcus aureus. Our results highlight the potential of G. simplicifolia phytochemicals in the development of functional foods, nutraceuticals, and dietary supplements.

HPLC-MS Analysis and evaluation of Antioxidant and Anti-Inflammatory Potential of Cinnamomum cassia Extract

HPLC-MS Analysis and evaluation of Antioxidant and Anti-Inflammatory Potential of Cinnamomum cassia Extract

Proso Millet (Panicum miliaceum L.) as Alternative Source of Starch and Phenolic Compounds: A Study on Twenty-Five Worldwide Accessions.

Proso millet has been proposed as an effective anti-diabetic food thanks to the combined action of polyphenols and starch. This study aimed to characterize the chemical composition of twenty-five accessions, in order to enhance this cereal as an alternative to available starch for food applications or to propose new food ingredients with health benefits. Proso millet contained a high percentage of starch, reaching values of 58.51%. The amylose content showed high variability, with values ranging from 1.36 to 42.70%, and significantly higher values were recorded for the white accessions than for the colored ones. High-resistant starch content (13.41-26.07%) was also found. The HPLC-MS analysis showed the same phenolic pattern in all the samples. Cinnamic acids are the most abundant compounds and significant differences in their total content were found (0.69 to 1.35 mg/g DW), while flavonoids were only detected in trace amounts. Statistical results showed significantly higher antiradical activity in the colored accessions than in the white ones.

Detoxification of aflatoxin B1 by Bacillus aryabhattai through conversion of double bond in terminal furan.

This study aimed to screen a bacterial strain with high detoxifying capability for aflatoxin B1 (AFB1), verify its biotransformation efficiency, and detoxification process. Three hundred and fifty samples collected from different environmental niche were screened using coumarin as the sole carbon source. HPLC was used to detect residues of AFB1, and 16S rRNA sequencing was performed on the isolated strain with highest AFB1 removal ratio for identification. The detoxified products of this strain were tested for toxicity in E. coli as well as LO2, Caco-2 and HaCaT human cell lines. HPLC-MS was applied to further confirm AFB1 removal and detoxification process. We identified a strain from plant leaf designated as DT with high AFB1-detoxifying ability that is highly homologous to Bacillus aryabhattai. The optimum detoxification conditions of this strain were 37°C and pH 8.0, resulting in 82.92% removal ratio of 2μg mL-1 AFB1 in 72h. The detoxified products were nontoxic for E. coli and significantly less toxic for the LO2, Caco-2 and HaCaT human cell lines. HPLC-MS analysis also confirmed the significant drop of the AFB1 characteristic peak. Two possible metabolic products, C19H15O8 (m/z 371) and C19H19O8 (m/z 375), were observed by mass spectrometry. Potential biotransformation pathway was based on the cleavage of double bond in the terminal furan of AFB1. These generated components had different chemical structures with AFB1, manifesting that the attenuation of AFB1 toxicity would be attributed to the destruction of lactone structure of AFB1 during conversion process.

Advanced technology for photocatalytic degradation of thiophanate-methyl: Degradation pathways, DFT calculations and embryotoxic potential

This study focuses on establishing an efficient two-step technology, which includes: (1) consecutive adsorption-desorption, using cellulose-based membranes, bCells, and (2) photocatalytic degradation of the fungicide thiophanate-methyl (TPM), using synthesized Ag-P25 and Ce-P25 catalysts. The catalysts, obtained by controlled deposition of Ag2O/Ag and CeO2 onto P25 TiO2 carrier (Degussa), were characterized using ATR-FTIR, XRPD, BET, FESEM, HRTEM, HAADF-EDS and UV–DRS techniques. In order to establish a feasible purification technology, preconcentration of TPM was performed by adsorption, achieving 75.5 and 92.9 mg/g of TPM removal using bCell-EpL and bCell–EpL–TA membranes, respectively, followed by efficient desorption (> 95%) that provided acceptable TPM concentration for photodegradation experiments. Under optimal conditions (0.07 g/L of both catalysts), complete degradation of TPM (5 mg/L) occurred within 2 h, compared to 4 h for the base TiO2 P25. Measurements of quantum yield and the results of HPLC-MS analysis, alongside DFT calculation, assisted in understanding the TPM degradation pathways. New degradation products were detected and proposed from HPLC–MS analysis. Embryotoxic assays, performed on zebrafish (Danio rerio), applied to estimate the toxicity evolution of time-dependent generated TPM degradation products, showed low embryotoxic potential. Chemical oxygen demand (26 mg O2/L) confirmed low ecotoxicological pressure of effluent water.

Unbiased and biased chemometric analysis of LC-MS data from human urine following coffee intake.

We carried out a human volunteer study with 14 participants, eight of whom were asked to consume one cup of coffee at four different time points. Urine samples were collected at eight time points and analyzed by HPLC-MS analysis. The LC-MS data were subjected to unsupervised multivariate statistical analysis (principal component analysis) followed by supervised multivariate analysis (linear discriminant analysis). In an unbiased approach, in the absence of data preselection and filtering, the most important features explaining differences between coffee consumers and the control group observed showed variations in endogenous human hormonal steroid metabolites as well as xanthine derivatives. Only after a biased data treatment data revealed differences between the sample groups based on literature reported chlorogenic acid metabolites resulting directly from coffee intake. Such analysis could confirm the presence of 21 previously reported chlorogenic acid plasma metabolites as urinary metabolites. The application of tandem MS molecular networking revealed the presence of five bioavailable chlorogenic acid derivatives in urine previously not reported, including both quinic acid lactone and dimethoxy caffeoyl esters. Selected cinnamic acids were quantified in urine.

Assessment of residues of fluchlordiniliprole in rice and its natural environmental matrices by QuEChERS method using HPLC-MS technique and dissipation behavior

Fluchlordiniliprole is a novel insecticide used to kill the rice stem borer (Chilo suppressalis). The concentrations of fluchlordiniliprole residue in the five objects of a pesticide-residue field trial (brown rice, rice husk, rice straw, paddy water, and paddy soil) were investigated by a combination of HPLC-MS and QuEChERS residue analysis. For the five field-trial objects, the LODs of fluchlordiniliprole ranged from 1.53 × 10-1 µg/kg to 7.00 × 10-1 µg/kg, the LOQs ranged from 5.11 × 10-1 µg/kg to 2.33 × 100 µg/kg, the fluchlordiniliprole standard curves showed good linearity (R2-values > 0.9997). The intra-day and the inter-day average percentage recoveries of fluchlordiniliprole and their RSD values were 90.3–117%, 91.2–116% and 1.77–4.35%, 1.73–4.20% respectively. These results indicated the high sensitivity, specificity, accuracy, and precision of the established analytical method. The dissipation of fluchlordiniliprole from paddy water, paddy soil, and rice straw followed first-order kinetics. The half-lives of fluchlordiniliprole in the three field-trial objects were less than 10 days, and the insecticide did not persist in any of the three objects after 75 days. This study concludes that fluchlordiniliprole is safe for the environment and supports the application of the insecticide in rice production around the world.

High temperature lacto-fermentation improves antioxidant and antidiabetic potentials of Lithuanian red beetroot

Diabetes is becoming a global pandemic and therefore calls for diverse therapeutic strategies for mitigating the disease. In this study, lactic acid bacteria isolated from Lithuanian traditional fermented foods were screened for β-Glucosidase activity and were used to ferment beetroot to develop an antidiabetic product. After fermentation, LAB PN39MY (also referred to as PN39) fermented samples demonstrated the strongest DPP-IV and α-Glucosidase inhibitory abilities of 50.0 ± 3.5% and 80.5 ± 5% respectively as well as the highest antioxidant capacity of 0.69 ± 0.04 mmol/L relative to all the other samples. Varying the fermentation conditions revealed that fermenting beetroot with PN39 at 45 °C for 72 h yielded the strongest DPP-IV and α-Glucosidase inhibition of 87.45% and 80.5 ± 5.3% respectively and increased the antioxidant capacity to 1.46 ± 0.01 mmol/L. Whole genome sequencing analysis of PN39 revealed the strain to be Latilactobacillus curvatus. HPLC-MS analysis of PN39 fermented samples showed that the fermentation process generated high levels of dihydromyricetin (an antidiabetic flavonoid) which was absent in unfermented beetroot. Results from this study indicate that fermenting beetroot with Latilactobacillus curvatus PN39 at 45 °C for 72 h would be an effective method for developing antidiabetic functional foods.

New Pseudomonas Bacterial Strains: Biological Activity and Characteristic Properties of Metabolites.

This paper investigates the antagonistic and plant growth promotion activity of the new indigenous bacteria antagonist strains P. chlororaphis BZR 245-F and Pseudomonas sp. BZR 523-2. It was found that on the 10th day of cultivation, BZR 245-F and BZR 523-2 exhibit an antagonistic activity against F. graminearum at the level of 59.6% and 15.1% and against F. oxysporum var. orthoceras at the level of 50.2% and 8.9%, respectively. Furthermore, the BZR 523-2 strain stimulated the growth of winter wheat seedlings more actively than the BZR 245-F strain. When processing seeds of winter wheat, Pseudomonas sp. BZR 523-2 indicators were higher than in the control: plant height increased by 10.3%, and root length increased by 18.6%. The complex characteristic properties of the metabolite were studied by bioautography and HPLC-MS. Bioautography proved the antifungal activity of phenazine nature compounds synthesized by the new bacterial strains. We qualitatively and quantitatively analyzed them by HPLC-MS analysis of the strain sample metabolites. In the BZR 245-F sample, we found more phenazine compounds of various types. Their total phenazine concentration in the BZR 245-F was more than five times greater than in the BZR 523-2. We defined crucial differences in the quantitative content of the other metabolites. Despite the difference between new indigenous bacteria antagonist strains, they can be used as producers of effective biopesticides for sustainable agriculture management.

Cobalt cross-linked ordered mesoporous carbon as peroxymonosulfate activator for sulfamethoxazole degradation

Ordered mesoporous carbons (OMCs) functionalized with catalytically-active metals have many potential applications in sulfate radical-based advanced oxidation processes for degrading antibiotics. Cobalt cross-linked ordered mesoporous carbon materials (OMC-Co-Tx) were synthesized through evaporation-induced self-assembly, calcinated at (600 to 800) oC. The OMC-Co-Tx materials were then employed as peroxymonosulfate (PMS) activators for removal of sulfamethoxazole (SMX) from aqueous solutions. OMC-Co-T800 prepared by calcination at 800 °C had a large specific surface area (449 m2/g), uniform pore structure (∼4.5 nm) and showed the best performance for activation of PMS. With a dosage of 0.1 g/L OMC-Co-T800 and 0.4 g/L PMS, the functionalized OMC material allowed SMX (10 mg/L) removal of up to 99% in 30 min. The increase of calcination temperature promoted the reduction of cobalt in OMC materials and increased the defects in their structure, resulting in better catalyst behavior. Quenching experiments and electron paramagnetic resonance analyses showed that reactive species of sulfamethoxazole degradation involved in the OMC-T800/PMS system were SO4•−, OH, O2•− and 1O2. HPLC-MS analyses of degradation intermediates formed in the OMC-Co-T800/PMS system allowed elucidation of four transformation pathways for SMX degradation.

Degradation of ciprofloxacin by persulfate activated by Fe(III)-doped BiOCl composite photocatalyst.

Fe-BOC-X photocatalyst was successfully prepared by solvothermal method. The photocatalytic activity of Fe-BOC-X was determined by ciprofloxacin (CIP), a typical fluoroquinolone antibiotic. Under sunlight irradiation, all Fe-BOC-X showed better CIP removal performance than original BiOCl. In comparison, the photocatalyst with iron content of 50 wt% (Fe-BOC-3) has excellent structural stability and the best adsorption photodegradation efficiency. The removal rate of CIP (10mg/L) by Fe-BOC-3 (0.6g/L) reached 81.4% within 90min. At the same time, the effects of photocatalyst dosage, pH, persulfate, persulfate concentration, and combinations of different systems (PS, Fe-BOC-3, Vis/PS, Vis/Fe-BOC-3, Fe-BOC-3/PS, and Vis/Fe-BOC-3/PS) on the reaction were systematically discussed. In reactive species trapping experiments, electron spin resonance (ESR) signals revealed that the photogenerated holes (h+), hydroxyl radical (•OH), sulfate radical (•SO4-), and superoxide radical (•O2-) played an important role in CIP degradation; hydroxyl radicals (•OH) and sulfate radicals (•SO4-) play a major role. Various characterization methods have demonstrated that Fe-BOC-X has larger specific surface area and pore volume than original BiOCl. UV-vis DRS indicate that Fe-BOC-X has wider visible light absorption and faster photocarrier transfer and provides abundant surface oxygen absorption sites for effective molecular oxygen activation. Accordingly, a large number of active species were produced and participated in the photocatalytic process, thus effectively promoting the degradation of ciprofloxacin. Based on HPLC-MS analysis, two possible decomposition pathways of CIP were finally proposed. The main degradation pathways of CIP are mainly due to the high electron density of piperazine ring in CIP molecule, which is mainly attacked by various free radicals. The main reactions include piperazine ring opening, decarbonylation, decarboxylation, and fluorine substitution. This study can better open up a new way for the design of visible light driven photocatalyst and provide more ideas for the removal of CIP in water environment.

Ultrasound enhanced destruction of tetracycline hydrochloride with peroxydisulfate oxidation over FeS/NBC catalyst: Governing factors, strengthening mechanism and degradation pathway

In this study, FeS/N-doped biochar (NBC) derived from the co-pyrolysis of birch sawdust and Mohr's salt was applied to evaluate the efficiency of catalyzed peroxydisulfate (PDS) oxidation for tetracycline (TC) degradation. It is found that the combination of ultrasonic irradiation can distinctly enhance the removal of TC. This study investigated the effects of control factors such as PDS dose, solution pH, ultrasonic power, and frequency on TC degradation. Within the applied ultrasound intensity range, TC degradation increases with increasing frequency and power. However, excessive power can lead to a reduced efficiency. Under the optimized experimental conditions, the observed reaction kinetic constant of TC degradation increased from 0.0251 to 0.0474 min−1, with an increase of 89%. The removal ratio of TC also increased from ∼85% to ∼99% and the mineralization level from 45% to 64% within 90 min. Through the decomposition testing of PDS, reaction stoichiometric efficiency calculation, and electron paramagnetic resonance experiments, it is shown that the increase in TC degradation of the ultrasound-assisted FeS/NBC-PDS system was attributed to the increase in PDS decomposition and utilization, as well as the increase in SO4•− concentration. The radical quenching experiments showed that SO4•−, •OH, and O2•− radicals were the dominant active species in TC degradation. TC degradation pathways were speculated according to intermediates from HPLC-MS analysis. The test of simulated actual samples showed that dissolved organic matter, metal ions, and anions in waters can undercut the TC degradation in FeS/NBC-PDS system, but ultrasound can significantly reduce the negative impact of these factors.

Investigation of Optical Properties and Activity of Wheat Stripe Rust Urediospores

Stripe rust is one of the most common diseases challenging the safe production of wheat. Rapid identification and analysis of urediospores, responsible for disease transmission, are the key to preventing and controlling stripe rust. The current spore detection is time-consuming and requires auxiliary equipment, but many optical detection methods and sensors with high efficiency, sensitivity, and detection ability have been developed and widely used. Thus, the investigation of optical parameters is the prerequisite for optical sensitive detection and is detailed in this study. Firstly, the microscopic images and surface elements of wheat stripe rust urediospores were obtained using a high-resolution electron microscope and an energy spectrum analyzer. The reflectivity and absorptivity spectra in the near-infrared band of active/inactivate urediospores were measured. Further, the optical parameters, such as reflection phase shift, complex refractive index, and dielectric constant, of the urediospores were analyzed based on electromagnetic theory and Kramers–Kronig relation. The results revealed that the urediospores have a strong tolerance to near-infrared light, and the real part of the complex refractive index n was between 1.0 and 1.4. These observations indicate that whether the spores are active or not has little effect on the real part and dielectric constant of the complex refractive index but has a significant impact on the imaginary part and extinction coefficient of the complex refractive index, and the corresponding relationship between the optical properties of urediospores and biological components was established. These findings were verified with HPLC-MS and Near-Infrared Spectroscopy Analysis Technology and lay a theoretical foundation for detecting urediospores of wheat stripe rust by using optical sensors. The study provides a reference for the analysis of optical characteristics of other biological samples.

Separation and characterisation of glyceryl glycosides and lignin from acid-catalysed glycerol pretreatment hydrolysate of sugarcane bagasse

Acid-catalysed glycerol (ACG) pretreatment of biomass is one of the pre-treating techniques for the enzyme-mediated lignocellulosic biorefinery, while inadequate attention has been paid to the glycerol modified saccharides and lignin redistributed to the hydrolysate, nor their bioactive properties. In this study, a sequential process involving tetrahydrofuran (THF) extraction and carbon/celite adsorption-elution was employed to recover lignin and glyceryl glycosides (GG) from ACG hydrolysate. The physicochemical and structural properties of lignin were systematically explored, and were related to their antioxidation properties, the composition and moisturising activities of GG was investigated. Two types of lignin i.e., water-insoluble lignin (WIL) and water-soluble lignin (WSL) were obtained, accounting for 49.60 wt% and 38.00 wt% of the total lignin in raw bagasse, respectively. GG separated from the hydrolysate yielded an overall recovery of 68.17 wt% of the xylan from the raw bagasse. The relatively high yield of lignin and GG can be attributed to the incorporation of glycerol molecules. 2D HSQC NMR results revealed that glycerol effectively preserved the β-O-4 structure of lignin during ACG pretreatment through α-etherification and γ-esterification. 31P NMR results showed that WSL has more aliphatic hydroxyl groups, resulting in increased water solubility, whereas WIL exhibited a higher amount of phenolic hydroxyl groups, contributing to the increased in vitro antioxidant properties. WSL contained significant proportion of p-coumaric acid glycerides and demonstrated low cytotoxicity along with a favorable cellular antioxidant capacity (CAA). HPLC-MS analysis revealed that the GG was a mixture of 56.44% glyceryl xylosides and 36.49% glyceryl glucosides, which displayed a superior moisturising capacity compared to commercial humectants such as hyaluronic acid (HA) and α-glyceryl glucosides (αGG). Overall, this study establishes a foundation for the extraction of value-adding bioactive compounds from acid-catalysed glycerol pretreatment hydrolysate, supporting the implementation of ACG techniques in biorefineries.

Isolation and Identification of Flavonoids from Black Cumin (Nigella sativa) by HPLC-MS and In Silico Molecular Interactions of Their Major Compounds with Fusarium oxysporum Trypsin-like Serine Protease

Fusarium oxysporum is one of the most harmful soil-borne pathogens that cause root rot, damping-off, and wilt disease in many plant species. Management of Fusarium oxysporum diseases is often by using many harmful and expensive chemical fungicides which have many harmful effects on the environment and human health. The current study was conducted to identify the chemical constituents of black cumin seeds’ methanolic extract and investigate the ability of the major constituents to inhibit the Fusarium oxysporum trypsin-like serine protease, which play an important role in F. oxysporun pathogenicity. The HPLC-MS analysis of black cumin seeds’ methanolic extract revealed the presence of seven major compounds: amentoflavone, Procyanidin C2, Quercetin3-O-sophoroside-7-O-rhamnoside, 5,7-Dihydroxy-3,4-dimethoxyflavone, Borapetoside A, tetrahydroxy-urs-12-en-28-O-[b-D-glucopyranosyl (1-2)-b-D-glucopyranosyl] ester, and kudzusapongenol A-hexA-pen. The results of molecular docking between these compounds and the active site of Fusarium oxysporium trypsin showed that only four compounds were able to bind to the active site of F. oxysporum trypsin. Amentoflavone, 5,7-Dihydroxy-3,4-dimethoxyflavone, and Quercetin3-O-sophoroside-7-O-rhamnoside have the highest binding energy, −6.4, −6.5, and −6.5 Kcal/mol, respectively. In addition, the results clarify that 5,7-Dihydroxy-3,4-dimethoxyflavone was the only compound to form a hydrogen bond with Asp189 (the residue responsible for substrate specificity). The results of the study strongly indicate that flavonoids of black cumin seeds’ methanolic extract could be used as effective inhibitors for the F. oxysporum trypsin-like serine protease.