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Combining anticancer drugs and phytomolecules with anticancer activity has opened up new avenues for cancer treatment and could be a potent alternative to conventional cancer therapy. Quercetin (QUR) and Erlotinib (ERB) exhibit potential anticancer properties. However, both drugs manifest low oral bioavailability due to low aqueous solubility, and interestingly, there is not a single validated UHPLC-PDA method for quantifying QUR and ERB simultaneously. Thus, the current study aims to address pharmaceutical challenges by encapsulating the two drugs in liquid crystalline nanoparticles (LCNPs) and to develop and validate a sensitive, accurate analytical, and bioanalytical method, as per guidelines, to quantify QUR and ERB simultaneously in LCNPs. Effective chromatographic elution of QUR and ERB has been achieved using a C8 reversed-phase column with an isocratic mobile phase at a flow rate of 1 mL/min, and both drugs were detected at 252 nm wavelength. The retention time was 5.3 and 7.7 min for QUR and ERB, respectively, while LOQ was less than 0.5 µg/mL for both drugs, appropriate for monitoring therapeutic drugs in preclinical and clinical research settings. The validated method was successfully applied to estimate the %drug entrapment efficiency, %drug loading, and %drug release for the simultaneous analysis of QUR and ERB in the LCNPs. The technique investigated both drugs' pharmacokinetic characteristics in Sprague–Dawley rats. The results were deemed reliable, and the validated method was found to be precise and accurate as per guidelines for the simultaneous estimation of QUR and ERB, which have applications in formulation development and bioanalytical studies. [ABSTRACT FROM AUTHOR]

In traditional Chinese medicine research, seaweeds used for drug and health food development mainly refer to Sargassum pallidum (Turn.) C. Ag. (SP) and Sargassum fusiforme (Harv.) Setch. (SF). In the Chinese Pharmacopoeia, polysaccharides are the main quality control indicators. The total sugar content is determined by the anthrone–sulfuric acid method to evaluate the quality of seaweeds. However, this method cannot reflect the structural characteristics of seaweed polysaccharides and cannot distinguish among different seaweed varieties. Given this, to comprehensively evaluate the quality of different seaweeds, this study conducted a thorough analysis of the primary structure of polysaccharides in 11 batches of SF and 7 batches of SP. The neutral sugar content was determined by the anthrone–sulfuric acid colorimetric method, weight average molecular weight (Mw) by high‐performance size exclusion chromatography coupled with multi‐angle laser light scattering and refractive index detector method, sulfate content by ion chromatography and monosaccharide composition by ultrahigh‐performance liquid chromatography method, while also using professional software for statistical and similarity analysis. The results showed significant differences (p < 0.05) in neutral sugar content and Mw between S. fusiforme polysaccharides and S. pallidum polysaccharides, which can be used to distinguish SF and SP. The monosaccharide composition fingerprint was analyzed using chemometric methods, and it was found that fucose and glucose could serve as differential markers to distinguish SF and SP. This study further deepens the understanding of polysaccharides in seaweeds and more comprehensively evaluates the quality of different seaweeds. [ABSTRACT FROM AUTHOR]

BACKGROUND: Protein hydrolysates (PHs) can enhance plant nitrogen nutrition and improve the quality of vegetables, depending on their bioactive compounds. A tomato greenhouse experiment was conducted under both optimal (14 mM) and suboptimal (2 mM) nitrogen (N‐NO3) conditions. Tomatoes were treated with a new Malvaceae‐derived PH (MDPH) and its molecular fractions (MDPH1, >10 kDa; MDPH2, 1–10 kDa and MDPH3, <1 kDa). RESULTS: Under optimal N conditions, the plants increased biomass and fruit yield, and showed a higher photosynthetic pigment content in leaves in comparison with suboptimal N, whereas under N‐limiting conditions, an increase in dry matter, soluble solid content (SSC) and lycopene, a reduction in firmness, and changes in organic acid and phenolic compounds were observed. With 14 mM N‐NO3, MDPH3 stimulated an increase in dry weight and increased yield components and lycopene in the fruit. The MDPH2 fraction also resulted in increased lycopene accumulation in fruit under 14 mM N‐NO3. At a low N level, the PH fractions showed distinct effects compared with the whole MDPH and the control, with an increase in biomass for MDPH1 and MDPH2 and a higher pigment content for MDPH3. Regardless of N availability, all the fractions affected fruit quality by increasing SSC, whereas MDPH2 and MDPH3 modified organic acid content and showed a higher concentration of flavonols, lignans, and stilbenes. CONCLUSION: The molecular weight of the peptides modifies the effect of PHs on plant performance, with different behavior depending on the level of N fertilization, confirming the effectiveness of fractioning processes. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

This study introduces a miniaturised solid-phase extraction (µ-SPE) method coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous quantification of 23 compounds, including psychoactive drugs, narcotics and their metabolites, in urine samples. The µ-SPE method, using standard laboratory equipment such as a centrifuge, was developed and validated, offering a practical and economical alternative to more traditional SPE methods. The key extraction parameters: elution solvent composition, sample and elution volumes, and sorbent mass were optimized to enhance performance. The method demonstrated high sensitivity, with detection limits between 0.06 and 0.41 ng cm−3 and quantification limits from 0.19 to 1.24 ng cm−3. The precision was confirmed with an intra-day precision ranging from 0.2% to 7.5% and an inter-day precision from 1.2% to 13.4%. Recovery rates ranged from 84.2% to 109.4%, with minimal matrix effects observed for most analytes (|ME|< 10%). The relative error remained below 5%, indicating good accuracy. The method was also evaluated in terms of greenness, practical, and analytical aspects using the WAC model. Based on the validation results, it was concluded that the developed method could be a good confirmatory method for results obtained by immunochemical tests and could also be used in both clinical analyses and forensic toxicology. [ABSTRACT FROM AUTHOR]

BACKGROUND RESULTS CONCLUSION Genetic breeding is essential to develop grapevine genotypes adapted to warm climates and resistant to pathogens. Traditionally cultivated Vitis vinifera is susceptible to biotic and abiotic stresses. Winemakers and consumers, however, perceive wines from non‐vinifera or hybrid cultivars as inferior. In this study, sensory analyses and comprehensive metabolite profiling by targeted and untargeted approaches were used to investigate the oenological potential of wines from grapes of genotypes developed throughout four breeding cycles to improve climate adaptation, sugar contents and berry color.Novel genotypes had higher yields and the wines exhibited increased contents of polyphenols, including anthocyanins. Volatile monoterpenes in the wines decreased throughout breeding cycles in the absence of selective pressure. Polyphenol contents were higher in intermediate wines, with hydroxytyrosol contents reaching up to three times reported values. Mouthfeel attributes astringency, leafy taste, flavor and body, and persistency showed significant correlation with untargeted features. Supervised model‐based analyses of the metabolome effectively discriminate wines from distinct genetic origins.Taken together, the results demonstrate the potential of novel grapevine genotypes to a more sustainable viticulture and quality wine production in warm climates. Comprehensive metabolite profiling of the wines reveals that genotype clustering is dependent on the chemical class and that traits not submitted to selective pressure are also altered by breeding. Supervised multivariate models were effective to predict the genetic origin of the wines based on the metabolic profile, indicating the potential of the technique to identify biomarkers for wines from sustainable genotypes. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Aim: Vildagliptin and Dapagliflozin in fixed-dose combination is used for treatment of Type II Diabetes Mellitus. The key objective of the current research work is to develop a new stability-indicating UHPLC method for the simultaneous estimation of Vildagliptin and Dapagliflozin in tablet dosage form as no such method is available. Materials and Methods: A successful separation was achieved by using Agilent column C18 (4.6×100 mm) and mobile phase of Methanol: 0.1% Orthophosphoric acid (78:22) at a flow rate of 1.0 mL and detection wavelength of 234 nm. The forced degradation study was performed at extreme forced conditions such as hydrolysis with acid and base, peroxide oxidation and photolytic degradation, following ICH guidelines. Results: The retention time for Vildagliptin and Dapagliflozin was 2.3 and 4.7 min respectively. The suggested approach yields linear responses for Vildagliptin and Dapagliflozin in the concentration of the 50-250 µg/mL and 5-25 µg/mL, respectively. Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 1.04 µg/mL and 3.15 µg/mL for Vildagliptin and 0.24 µg/mL and 0.73 µg/mL for Dapagliflozin, respectively. In the exposed conditions, the drugs did not exhibit any significant degradation. Conclusion: The UHPLC approach that was recommended proved to be highly sensitive, accurate, precise, robust and stability indicating. The method can be successfully adopted for the routine analysis for the simultaneous estimation of the Vildagliptin and Dapagliflozin in bulk and pharmaceutical dosage form. [ABSTRACT FROM AUTHOR]

Introduction: Despite numerous successful cases, there are still some challenges in using analytical quality by design (AQbD) for the development of analytical methods. Knowledge organization helps to enhance the objectivity of risk assessment, reduce the number of preliminary exploratory experiments, identify potential critical method parameters (CMPs) and their scope. Objective: In the present study, we aimed to develop a simple, rapid, and robust analytical method for detecting phenolic compounds in Xiaochaihu capsule intermediates utilizing knowledge organization. Methods: Knowledge organization and AQbD were combined to obtain the initial analytical conditions through knowledge collection, extraction, reorganization, and analysis. The quantitative relationship between critical method attributes (CMAs) and CMPs was then established by a definitive screening design. The method operable design region was calculated using an exhaustive Monte Carlo approach based on the probability of reaching the standard. Robustness investigation and methodological validation were finally performed. Results: Analytical target profiles, CMAs, potential CMPs, and initial analytical conditions were initially identified, and the optimized ranges of operating parameters were obtained. A UHPLC method was successfully established for the analysis of phenolic compounds in ginger–ginger pinellia percolate, and the method validation outcomes were also satisfactory. Conclusion: The developed method can be a reliable means to detect the phenolic compounds of Xiaochaihu capsule intermediates. Knowledge organization provides a new approach for making better use of prior knowledge, significantly enhancing the efficiency of analytical method development. The approach is versatile and can be similarly applied to the development of other methods. This study employed an AQbD process based on knowledge organization to develop an analytical method for detecting phenolic compounds in Xiaochaihu capsule intermediate, improving the efficiency of conducting single‐factor experiments and identifying potential CMPs in the early stage of method development. Simultaneously, it offers a new approach for utilizing prior knowledge effectively. This analytical method can be used for quality control of intermediate in Xiaochaihu capsule. [ABSTRACT FROM AUTHOR]

Vitis vinifera L. is a natural source of bioactive compounds that is already used for cosmeceutical and nutraceutical approaches. However, their phytochemical and antioxidant properties, although studied, have not been fully explored. We aimed to characterize V. vinifera L. cv. Falanghina seed extracts in different polarity solvents (hexane, ethyl acetate, ethanol, and a mixture of acetone–water) for their phytochemical contents, including the total phenolic compound content (TPC), free radical scavenging capacities, and antioxidant ability on HepG2 cells. We directly profiled the functional quality of V. vinifera seed extracts against H2O2-induced oxidative stress in HepG2 cells, focusing on mitochondrial functions. The content of bioactive compounds was characterized by LC-MS. To assess the cytocompatibility of the extracts, a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay was conducted. Results showed that extraction with ethyl acetate (18.12 mg GAE·g−1) and ethanol solvents (18.07 mg GAE·g−1), through Soxhlet, and with an acetone–water mixture (14.17 mg GAE·g−1), through maceration, yielded extracts rich in (poly)phenols, with good scavenging and antioxidant activity (98.32 I% for ethanol solvents and 96.31 I% for acetone–water mixture). The antioxidant effect of polyphenols is at least partially due to their capacity to maintain mitochondrial biogenesis and mitophagy, which elevates mitochondrial efficiency, resulting in diminished ROS production, hence re-establishing the mitochondrial quality control. These findings highlight the valorization of Vitis by-products to improve food functional characteristics. [ABSTRACT FROM AUTHOR]

Summary: Herein, an ultra‐high performance liquid chromatography coupled to a diode array detector (UHPLC‐DAD) based quantification method has been developed for the simultaneous determination of 21 bioactive phenolic compounds present abundantly in food products. The developed method was validated in terms of parameters such as linearity, detection and quantification limits, intra‐day and inter‐day precision and recovery showing ideal results. Further, the developed method was applied for the quantitative analysis of phenolics in commercially procured dietary samples such as spices, green tea, black tea and dark chocolate. The major phenolics quantified in dry weight of different samples were epigallocatechin gallate (425.5 mg/10 g), epicatechin gallate (111.9 mg/10 g) in green tea; gallocatechin (286.8 mg/10 g) in dark chocolate; and naringin (93.9 mg/10 g) in star anise etc. Overall, the UHPLC‐DAD‐based method was found to be reliable, simple and specific for the estimation of phenolics in different targeted food samples. [ABSTRACT FROM AUTHOR]

Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants (POPs) that are widely distributed in the environment and cause significant environmental damage. Furthermore, they endanger human health by polluting food from the natural environment and food processing. Therefore, it is necessary to accurately detect PAHs in various sample matrices, which requires precise, practical, and rapid detection methods. The purpose of this research is to develop a high sensitivity analysis method by analyzing the optimum excitation and emission wavelengths of EPA's 15 priority polyaromatic hydrocarbons in the UHPLC fluorescence detector (Acenaphthene, Anthracene, Benzo[a]anthracene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Benzo[ghi]perylene, Benzo[a]pyrene, Chrysene, Dibenzo[a,h]anthracene, Fluoranthene, Fluorene, Indeno[1,2,3-cd]pyrene, Naphthalene, Phenanthrene, and Pyrene). An average of 17–25 analyses were performed for each polyaromatic hydrocarbon, and optimized excitation and emission wavelengths were obtained. LOD levels between 2 and 90 ppt were obtained with the method created in this direction. It is worth mentioning that the limits achieved for some PAH parameters are lower than those reported in the literature after pre-concentration steps. [ABSTRACT FROM AUTHOR]

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Abstract More catechins are found in green tea than in any other type of tea, with its predominant production taking place in Asian nations. Consumption of green tea has been strongly correlated with a reduced risk of many diseases. This study introduces a new, efficient, and reliable method for extracting total catechins using ultra-high-performance liquid chromatography coupled with an ID-X-Orbitrap Mass spectrometer (UHPLC-IDX-Orbitrap-MS). The method was then applied to quantify the catechin content in green tea, yielding results comparable to previously published studies. Among the various sources of green tea analyzed, the lowest average catechin content was observed in Vietnam, Japan (2: Matcha), and Morocco, ranging between 346 and 322 mg/L. Conversely, the highest average catechin content (between 424 and 422 mg/L) was found in Sri Lanka and Japan (1: Sencha). For the remaining green tea extracts, the catechin levels ranged from 367 to 410 mg/L, exhibiting similar values. These findings demonstrate the high reproducibility of the proposed extraction procedure, with a relative standard deviation (RSD) error of less than 15% for the catechin standard. Additionally, the limit of detection for catechins was determined to be 1 ng mL-1. This study serves as a pilot investigation for extracting catechins from various green tea sources. Future research will focus on identifying all active compounds present. Furthermore, it is worth noting that this study aligns with the goals set forth in Saudi Vision 2030, which aims to diversify the country's economy and promote scientific advancements in various fields, including healthcare and agriculture.

Aflatoxins (AFs) are a group of mycotoxins produced by certain fungi of Aspergillus spp. AFs of major concern are B1 (AFB1), B2 (AFB2), G1 (AFG1), G2 (AFG2), and M1 (AFM1). AFM1 is a hydroxylated metabolite of AFB1 formed inside the animal's body which is excreted into milk of cows that consumed AFB1 contaminated feed. Consumption of AFM1-contaminated milk and subsequent dairy products causes negative health effects in consumers. This study was conducted to determine the occurrence and levels of AFM1 in cheese products available in the Sri Lankan market where AFM1 is not regularly monitored in milk while having an outdated regulatory limit of 1 ppb established for dairy products. Processed cheese (n = 28), hard cheese (n = 14), semi-hard cheese (n = 5), and soft cheese (n = 3) representing seven popular brands were collected. The samples were analyzed by Ultra High-Performance Liquid Chromatography Fluorescence Detection. AFM1 was detected in 40 samples (80 %), while 17 (34 %) and 37 (74 %) of the samples had AFM1 levels exceeding the maximum permitted limit set by Codex Alimentarius Commission (0.5 ppb) and the Netherlands (0.2 ppb). Further, 10 samples violated the Sri Lankan maximum limit of 1 ppb. Thirteen out of the 14 hard cheese (92.9 %, 0.11–14.43 ppb) and all semi-hard cheese samples (100 %, 0.29–0.65 ppb) contained AFM1. Most of the soft (66.7 %, 0.35–0.45 ppb) and processed (71.4 %, 0.11–1.35 ppb) cheese samples had AFM1. Most of the locally manufactured cheese products in Sri Lankan market may pose health risks to consumers. The results highlight the significance of regular monitoring of AFM1 in dairy products and the importance of updating regulations on par with international standards concurrently to ensure consumer safety.

A novel green ultra high performance liquid chromatography (UHPLC) method was validated and estimated the measurement uncertainty for simultaneous determination of metoprolol tartrate (MET) and hydrochlorothiazide (HCT) in binary tablet. A Zorbax® SB-C18 column with isocratic elution (flow rate 0.9 mL min−1) at 25°C was used. Analytes and HCT degradation product were separated in approximately 1 min using acetonitrile:water:triethylamine (17:83:0.2, v/v) as mobile phase. Analytical curves were linear with (R2 > 0.99 for MET and HCT) with detection limits of 2.42 and 1.05 µg mL−1 for MET and HCT, respectively. Precision measurements showed RSD% from 0.39 to 1.2% and method accuracy by recovery tests was 100 ± 2%. Measurement uncertainties using Eurachem procedure were 100.1 ± 2.8% and 100.3 ± 2.4% for MET and HCT, respectively. This UHPLC method was accurate, precise, linear and selective, making it suitable for pharmaceutical quality control. It also proved eco-friendly compared to other reported methods.

Molnupiravir, a promising antiviral agent, has gained significant attention for its potential in treating viral infections, particularly in the context of the coronavirus disease 2019 pandemic. This study aimed to develop and validate an ultra‐high‐performance liquid chromatography (UHPLC) method for the quantification of Molnupiravir and its associated impurities (Imp‐I, Imp‐II, Imp‐III, and Imp‐IV). The method involved a systematic investigation of critical method parameters and their optimization using Quality by Design principles. The percentage of organic modifiers, column temperature, and flow rate were systematically optimized using the Box‐Behnken design. The developed method was assessed for specificity, system suitability, accuracy, precision, linearity, and detection limits. The results demonstrate strong specificity, with the analysis remaining accurate even in the presence of impurities. The developed method exhibits excellent precision, with repeatability and intermediate precision showing relative standard deviation values ranging from 0.78% to 1.14% for impurities and 0.82% to 1.91% for Molnupiravir. Furthermore, the method displays exceptional linearity, covering a wide range of concentrations. The linear regression analysis yields high coefficients of determination (r2, 9993–0.9997), confirming the linearity. The developed UHPLC method is well‐suited for the accurate and reliable analysis of Molnupiravir and its impurities, making it a valuable tool for quality control and pharmaceutical research applications. [ABSTRACT FROM AUTHOR]

Objectives: To develop and validate a sensitive, accurate, simple, precise and cost-effective UHPLC method for the simultaneous determination of Teneligliptin and Pioglitazone in pure and its tablet formulation form and validating this developed method as per Guidelines of ICH (Figure 1). Materials and Methods: The chromatographic separation was done by using column Agilent C18 (2.5 µm; 4.6x100 mm ID), isocratic mobile phase consists of Methanol: 0.1% TEA (PH-6 WITH OPA) 60: 40%v/v. The flow rate of mobile phase is 0.9 mL/min. The separation was carried out at 241 nm wavelength. The current method for accuracy, precision, linearity, specificity, robustness and ruggedness was validated as per ICH guidelines. Results: Teneligliptin and Pioglitazone retention time observed at 2.382 and 3.315 min respectively. The graphs showing peak area against concentration demonstrated linear between 2-10 µg/mL for Teneligliptin and 1.5-7.5 µg/mL for Pioglitazone. This relationship exhibited a high level of linearity with a Regression coefficient (R2) of 0.999. The determined limit of detection is 0.0843 and 0.0084 µg/mL while the limit of quantification was found to be 0.255 and 0.025 µg/mL for Teneligliptin and Pioglitazone respectively. The assay percentage of the available formulation was found to be 99.72 and 100.51 for Teneligliptin and Pioglitazone. Conclusion: The Validation parameters indicate the effective separation of the drug substance from their degradants effectively. This developed method shows the suitability for the routine quantitative analysis of Teneligliptin and Pioglitazone in its pure and their available pharmaceutical formulations for quality control purpose. [ABSTRACT FROM AUTHOR]

The technology of ultrahigh performance liquid chromatography (UHPLC) and ion chromatography (IC) with valve switching method is suitable for the simultaneous analysis of samples containing organic compounds and inorganic anions, which simplifies the pretreatment process, eliminates the complex matrix, enriches inorganic anions, realizes the simultaneous analysis of organic compounds and inorganic anions, and improves the efficiency of chromatographic analysis. The technology of ultrahigh performance liquid chromatography and ion chromatography with valve switching method is introduced into the undergraduate instrument analysis experiment class, which deepens the students' understanding of the special advantages of the new technology, improves the undergraduates' ability to solve complex practical problems, widens the field and enriches the content of instrument analysis experiment. Of course, it is conducive to the cultivation of innovative and comprehensive talents. [ABSTRACT FROM AUTHOR]

Oxalic acid and its salts, oxalates, are end products of metabolism found widely in plant kingdom. Once consumed, these compounds can bind with calcium, to form calcium oxalate stones, the most common types of kidney stone. Oxalate oxidase (OxO), an oxalate-degrading enzyme, is produced by the metabolic activities of microorganisms or plants, especially during the germination of cereal grains. The purpose of this study was to investigate impacts of extraction conditions on the OxO activity of germinated paddy rice (Oryza sativa L.) using Ultra-high performance liquid chromatography. The effects of three factors namely pH (2–7), solvent-to-sample ratios (3:1–8:1 v/w), and extraction time (15–75 min) were investigated. The results showed that the activity was higher at more acidic pH, ranging from 2 to 4. In addition, the OxO activity rose as the solvent-to-sample ratios increased and reached a peak at the ratio of 5:1 before dropping rapidly. Prolonging extraction times, from 15 to 60 min, resulted in increases in the OxO activity. [ABSTRACT FROM AUTHOR]

BACKGROUND: Yield, disease tolerance, and climate adaptation are important traits in grapevine genetic breeding programs. Selection for these characteristics causes unpredictable changes in primary and specialized metabolism, affecting the physicochemical properties and chemical composition of the berries and their processed products, juice, and wine. In this study, we investigated the influence of the genetic distance between grapevine genotypes on the chemical signatures of the juices, by integrating comprehensive metabolic profiling to genetic analyses. RESULTS: The studied grapevine cultivars exhibited low genetic diversity. Breeding for agronomic traits promoted higher contents of soluble sugars, total phenolics, and anthocyanins in the juices. Untargeted juice metabolomics identified a total of 147 metabolites, consisting of 30 volatiles, 21 phenolics, and 96 ultra‐high‐performance liquid chromatography–mass spectrometry (UHPLC‐MS) features. Juices from grapes of the most recent cultivars exhibited increased levels of trans‐resveratrol, catechin, and luteolin. The blend of volatiles from juices of later cultivars was also more complex, consisting of 29 distinct metabolites in 'BRS Magna'. Grapes from 'BRS Carmem', an intermediate cultivar, gave the most divergent UHPLC‐MS juice profile. CONCLUSION: Contents of soluble solids, total phenolics, and anthocyanins in grape juices were increased by controlled crosses and hybrid selection. Integrative analyses demonstrated that the juices' metabolic profiles accurately represent the cultivars' genetic distances. Juices from 'BRS Violeta' and 'BRS Magna' show relevant positive association with health‐related phenolics and a distinct set of odor volatiles, although these characteristics were specifically sought by breeding. © 2023 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Harmful algal blooms kill fish populations worldwide, as exemplified by the haptophyte microalga Prymnesium parvum. The suspected causative agents are prymnesins, categorized as A-, B-, and C-types based on backbone carbon atoms. Impacts of P. parvum extracts and purified prymnesins were tested on the epithelial rainbow trout fish gill cell line RTgill-W1 and on the human colon epithelial cells HCEC-1CT. Cytotoxic potencies ranked A > C > B-type with concentrations spanning from low (A- and C-type) to middle (B-type) nM ranges. Although RTgill-W1 cells were about twofold more sensitive than HCEC-1CT, the cytotoxicity of prymnesins is not limited to fish gills. Both cell lines responded rapidly to prymnesins; with EC50 values for B-types in RTgill-W1 cells of 110 ± 11 nM and 41.5 ± 0.6 nM after incubations times of 3 and 24 h. Results of fluorescence imaging and measured lytic effects suggest plasma membrane interactions. Postulating an osmotic imbalance as mechanisms of toxicity, incubations with prymnesins in media lacking either Cl−, Na+, or Ca2+ were performed. Cl− removal reduced morphometric rearrangements observed in RTgill-W1 and cytotoxicity in HCEC-1CT cells. Ca2+-free medium in RTgill-W1 cells exacerbated effects on the cell nuclei. Prymnesin composition of different P. parvum strains showed that analog composition within one type scarcely influenced the cytotoxic potential, while analog type potentially dictate potency. Overall, A-type prymnesins were the most potent ones in both cell lines followed by the C-types, and lastly B-types. Disturbance of Ca2+ and Cl− ionoregulation may be integral to prymnesin toxicity. [ABSTRACT FROM AUTHOR]

Honey bee pollen (HBP) is a hive product produced by worker bees from floral pollen grains agglutination. It is characterized by its excellent nutritional and bioactive composition, making it a superior source of human nutrition. This study aimed to evaluate the monofloral bee pollen samples, including Cistus, Crataegus monogyna, Cyanus, Elaeagnus angustifolia, Papaver somniferum, Quercus, Salix, Sinapis, and Silybum from Türkiye according to palynological analysis, antioxidant activity, phenolic profiles, and color. The phenolic profiles were detected using ultra‐high performance liquid chromatography coupled with tandem mass spectrometry. Bee pollens were categorized into monofloral, bifloral, and multifloral, underscoring the significance of confirming the botanical source of them depending on palynological analyses. Total phenolic content (TPC) of bee pollens ranged from 4.5 to 14.4 mg gallic acid/g HBP. The samples exhibited antioxidant activity for 2,2′‐azinobis‐(3‐ethylbenzothiazoline‐6‐sulfonic acid) (ABTS •+) ranging from 94.9 to 233.5 µmol trolox/g HBP, whereas lower values were seen for 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH•) ranging from 25.86 to 70.81 µmol trolox/g HBP. A yellowish‐red tint color was also displayed for whole samples, whereas only E. angustifolia bee pollen indicated a darker color (L* = 31.6). Among the phenolic compounds, luteolin, kaempferol, isorhamnetin, rutin, and genistein were the most abundant, and their profiles varied across the samples. It was also observed that TPC, antioxidant activities, and polyphenol composition were higher in samples containing pollen grains of P. somniferum, Quercus, Plantago, and E. angustifolia species. Practical Application: The increasing number of new findings on honey bee pollen is crucial to food science and technology. In this sense, this study offers a robust method for verifying the authenticity and quality of 11 monofloral bee pollens, which is crucial for the food industry. It also identifies potential sources of high‐quality pollen, benefiting producers, and consumers seeking superior bee pollen products. [ABSTRACT FROM AUTHOR]

The present study compared the performance of Ultra-high performance liquid chromatography (UHPLC) and UV–Vis spectrophotometry for the quantification of metformin hydrochloride in five commercially available metformin hydrochloride products with different strengths. The metformin hydrochloride was measured in the UHPLC with a mobile phase consisting of a mixture of 0.05 M phosphate buffer solution and methanol (35:65, v/v) with a pH of 3.6. Metformin hydrochloride was determined spectrophotometrically at 234 nm using a mixture of methanol and water as a blank. The methods’ linearity for metformin hydrochloride was within the concentration range of (2.5–40 μg/ml) in both techniques. The validation process encompassed assessments of specificity, selectivity, linearity, accuracy, precision, the lower limit of quantification (LLOQ), the lower limit of detection (LLOD), robustness, and system suitability. For the UHPLC validation method, the repeatability and reproducibility (expressed as relative standard deviation) were less than 1.578 and 2.718 %, respectively. The LLOQ for metformin hydrochloride was 0.625 μg/ml, and the LLOD was 0.156 μg/ml. For the UV–Vis spectrophotometric validation method, the repeatability and reproducibility (stated as relative standard deviation) were less than 3.773 and 1.988 %, respectively. The percentage recovery results for the five brands of metformin hydrochloride tablets were (98–101 %) and (92–104 %) for the UHPLC and UV–Vis spectrophotometric methods, respectively. In conclusion, the described methodologies were successfully employed for the quantitative analysis of metformin hydrochloride in different pharmaceutical tablet products.

Recently, concern about the environmental impact of drug analysis methods has increased significantly. Reversed-phase high-performance liquid chromatography (RP-HPLC), the predominant technique in drug analysis, relies heavily on organic solvents such as acetonitrile, which is known for its chromatographic efficiency, but also for its toxicity and flammability. To address these concerns, it is essential to minimize the use of toxic organic solvents. The aim of this study is to explore greener RP-HPLC modifications and evaluate their applicability in the pharmaceutical industry. Methods were developed for the separation of dronedarone hydrochloride and its degradation products based on experimental design, including micellar liquid chromatography (MLC), b-cyclodextrin (CD) modified RP-HPLC and ultra-high performance liquid chromatography (UHPLC). The eco-friendliness of these methods was assessed using the analytical eco-scale score, green analytical procedure index (GAPI) and analytical greenness (AGREE). AGREE appears to be the most suitable, as it revealed the greatest differences between the compared methods, as well as insights into critical aspects of the methods. UHPLC and b-CD modified RP-HPLC have been shown to be superior to MLC, and both methods can be a good choice, depending on whether the ease of implementation or energy efficiency is considered to be a more important criterion.

Buds of poplar trees (Populus species) are often covered with sticky, usually polyphenol-rich, exudates. Moreover, accessible data showed that some Populus bud extracts may be excellent antibacterial agents, especially against Gram-positive bacteria. Due to the fragmentary nature of the data found, we conducted a systematic screening study. The antimicrobial activity of two extract types (semi-polar—ethanolic and polar—ethanolic-water (50/50; V/V)) from 27 bud samples of different poplar taxons were compared. Antimicrobial assays were performed against Gram-positive (five strains) and Gram-negative (six strains) bacteria as well as fungi (three strains) and covered the determination of minimal inhibitory, bactericidal, and fungicidal concentrations. The composition of extracts was later investigated by ultra-high-performance liquid chromatography coupled with ultraviolet detection (UHPLC-DAD) and with electrospray-quadrupole-time-of-flight tandem mass spectrometry (UHPLC-ESI-qTOF-MS). As a result, most of the extracts exhibited good (MIC ≤ 62.5 µg/mL) or moderate (62.5 < MIC ≤ 500 µg/mL) activity against Gram-positives and Helicobacter pylori, as well as fungi. The most active were ethanolic extracts from P. trichocarpa, P. trichocarpa clone 'Robusta', and P. tacamahaca × P. trichocarpa. The strongest activity was observed for P. tacamahaca × P. trichocarpa. Antibacterial activity was supposedly connected with the abundant presence of flavonoids (pinobanksin, pinobanksin 3-acetate, chrysin, pinocembrin, galangin, isosakuranetin dihydrochalcone, pinocembrin dihydrochalcone, and 2′,6′-dihydroxy-4′-methoxydihydrochalcone), hydroxycinnamic acids monoesters (p-methoxycinnamic acid cinnamyl ester, caffeic acid phenethylate and different isomers of prenyl esters), and some minor components (balsacones). [ABSTRACT FROM AUTHOR]

Ligustrum vulgare (LV), widely cultivated in Europe and often used in hedges, has been historically recognized in folk medicine for its potential health benefits. This study focused on exploring the untargeted identification of secondary metabolites in ethanol extracts (70% v/v) from different morphological parts (young shoots, leaves, flowers and fruits) of LV at various stages of plant development, using ultra-high-performance liquid chromatography with high-resolution mass spectrometry (UHPLC-HRMS). Additionally, the selected biological activities (antioxidant activity, cyclooxygenase-2 inhibition (COX-2), α-amylase inhibition and cytotoxicity) of the tested extracts were determined. Untargeted metabolomics showed that LV extracts were a rich source of phenylethanoid compounds, flavonoids, iridoids and their derivatives. The flowers of LV had the highest content of oleuropein (33.43 ± 2.48 mg/g d.w.). The lowest antioxidant activity was obtained for ripe and post-seasonal fruits, while in the case of other samples, the activity was at a similar level. All tested extracts showed α-amylase and COX-2 inhibitory activity. In addition, LV extracts showed strong antiproliferative properties in colorectal (HT29) and liver (HepG2) cancer cell lines. The obtained results show the difference in the content of bioactive compounds in various morphological parts of Ligustrum vulgare. These differences may influence the multifaceted medicinal potential of this plant. [ABSTRACT FROM AUTHOR]

Why was the work done: The incorporation of unmalted barley at high proportion in the grist can introduce unfavourable bitter and astringent characteristics to beer, resulting in an upper limit on the proportion used. The flavour active compounds from raw barley which contribute these characteristics to the beer remain to be identified. How was the work done: This study used non-targeted metabolomics to determine non-volatile metabolites which could contribute to flavour differences when brewing with barley. Three beers were analysed using ultra-high performance liquid chromatography (UHPLC) coupled to a quadrupole time-of-flight mass spectrometer (qTOF) with an electro-spray ionisation source (ESI). One beer was produced using 100% malt and two beers with a grist of 15% barley and 85% malt (beers A and B). The barley was used untreated (beer A) or treated using a proprietary process (beer B). The metabolomic profiles of the three beers were compared and statistically different molecular features were annotated via analysis of MS2 spectra. What are the main findings: Several of the main differential molecular features were nitrogenous peptides and purine derivatives. This was attributed to the lack of the malting process and associated proteolytic enzyme activity reducing the extent of protein and peptide breakdown in the unmalted barley. Several of the identified peptides had amino acid residues which are known to cause bitter and kokumi (rich) taste in beer, which could explain the bitterness when brewing with unmalted barley. Why is the work important: A non-targeted approach offers new insights into non-volatile molecular features in beer that have not been previously identified with targeted analyses. Accordingly, this work identifies metabolites and groups of compounds which have not been previously considered when investigating the unfavourable bitterness and astringency associated with the use of unmalted barley. [ABSTRACT FROM AUTHOR]

A novel green ultra high performance liquid chromatography (UHPLC) method was validated and estimated the measurement uncertainty for simultaneous determination of metoprolol tartrate (MET) and hydrochlorothiazide (HCT) in binary tablet. A ZorbaxR SB-C18 column with isocratic elution (flow rate 0.9 mL min−1) at 25°C was used. Analytes and HCT degradation product were separated in approximately 1 min using acetonitrile:water:triethylamine (17:83:0.2, v/v) as mobile phase. Analytical curves were linear with (R² > 0.99 for MET and HCT) with detection limits of 2.42 and 1.05 µg mL−1 for MET and HCT, respectively. Precision measurements showed RSD% from 0.39 to 1.2% and method accuracy by recovery tests was 100 ± 2%. Measurement uncertainties using Eurachem procedure were 100.1 ± 2.8% and 100.3 ± 2.4% for MET and HCT, respectively. This UHPLC method was accurate, precise, linear and selective, making it suitable for pharmaceutical quality control. It also proved eco-friendly compared to other reported methods. [ABSTRACT FROM AUTHOR]

The presence of insecticide residues in chilli fruits limits the export and poses a health risk to consumers. Thus, it is necessary to develop quick and effective methods for conducting residue analysis of commonly used insecticides. The present research validates a modified QuEChERS technique for analysing thiacloprid and emamectin benzoate residues in chilli using UHPLC. The proposed methods recovered thiacloprid and emamectin benzoate by 80.33-88% and 79.33-96%, respectively. LOQ for both the insecticides was 0.01 mg/kg. Matrix effect values were within an acceptable range of -20 to 20%. The developed methodology can be used for periodical monitoring of the residue levels of the target insecticides in chilli. [ABSTRACT FROM AUTHOR]

Diterpenes from the Euphorbia genus are known for their ability to regulate the protein kinase C (PKC) family, which mediates their ability to promote the proliferation of neural precursor cells (NPCs) or neuroblast differentiation into neurons. In this work, we describe the isolation from E. resinifera Berg latex of fifteen 12-deoxyphorbol esters (1–15). A triester of 12-deoxy-16-hydroxyphorbol (4) and a 12-deoxyphorbol 13,20-diester (13) are described here for the first time. Additionally, detailed structural elucidation is provided for compounds 3, 5, 6, 14 and 15. The absolute configuration for compounds 3, 4, 6, 13, 14 and 15 was established by the comparison of their theoretical and experimental electronic circular dichroism (ECD) spectra. Access to the above-described collection of 12-deoxyphorbol derivatives, with several substitution patterns and attached acyl moieties, allowed for the study of their fragmentation patterns in the collision-induced dissociation of multiple ions, without precursor ion isolation mass spectra experiments (HRMSE), which, in turn, revealed a correlation between specific substitution patterns and the fragmentation pathways in their HRMSE spectra. In turn, this allowed for a targeted UHPLC-HRMSE analysis and a biased non-targeted UHPLC-HRMSE analysis of 12-deoxyphorbols in E. resinifera latex which yielded the detection and identification of four additional 12-deoxyphorbols not previously isolated in the initial column fractionation work. One of them, identified as 12-deoxy-16-hydroxyphorbol 20-acetate 13-phenylacetate 16-propionate (20), has not been described before. [ABSTRACT FROM AUTHOR]

Understanding the metabolism of pharmaceutical compounds is a fundamental prerequisite for ensuring their safety and efficacy in clinical use. However, conventional methods for monitoring drug metabolism often come with the drawbacks of being time-consuming and costly. In an ongoing quest for innovative approaches, the application of electrochemistry in metabolism studies has gained prominence as a promising approach for the synthesis and analysis of drug transformation products. In this study, we investigated the hepatic metabolism of voriconazole, an antifungal medication, by utilizing human liver microsomes (HLM) assay coupled with LC-MS. Based on the obtained results, the electrochemical parameters were optimized to simulate the biotransformation reactions. Among the various electrodes tested, the chemometric analysis revealed that the iron(II) phthalocyanine electrode was the most effective in catalyzing the formation of all hepatic voriconazole metabolites. These findings exemplify the potential of phthalocyanine electrodes as an efficient and cost-effective tool for simulating the intricate metabolic processes involved in drug biotransformation, offering new possibilities in the field of pharmaceutical research. Additionally, in silico analysis showed that two detected metabolites may exhibit significantly higher acute toxicity and mutagenic potential than the parent compound. [ABSTRACT FROM AUTHOR]

Abstract Background Sofosbuvir/ledipasvir (SOF/LDV), a combination of antiviral drugs, has been recently repurposed for COVID-19 management, according to Food and Drug Administration approval. Paracetamol (PAR) identified as a first-line antipyretic for COVID-19 symptoms' management. The use of these three drugs together has significantly influenced the management of COVID-19 by providing symptomatic relief via inhibiting viral activity. A validated ultra-high performance liquid chromatographic (UHPLC) method has been introduced for the quantification of these repurposed drugs in COVID-19 treatment. This novel chromatographic method allows the simultaneous detection of SOF, LDV, and PAR in bulk. Additionally, the method has been applied to determine the levels of SOF and LDV in human plasma samples with PAR used as an internal standard. Results A new UHPLC method was developed, using a mobile phase with a combination of acetonitrile and 0.1% orthophosphoric acid in a proportion of 42:58 (v/v).Flow rate was set at 0.4 ml/min, and UV detection was adjusted at 254 nm. The concentration of SOF, LDV, and PAR were measured by their corresponding peak areas, and showed linear relationships between concentration and peak area within the ranges of (5–60) µg/ml for SOF, (2–22) µg/ml for LDV, and (1–22) µg/ml for PAR. The presented UHPLC method was used to quantify the amounts of SOF, LDV, and PAR in both bulk samples and human plasma samples being spiked with the mentioned analytes. The elution process was completed within 4 min, with retention times of 3.28 min for SOF, 2.28 min for LDV, and 1.70 min for PAR. The method showed high separation selectivity, with an injection volume of 1µl. The precision, accuracy and repeatability of the method were found to be within acceptable limits. Conclusion The recently developed method has been successfully validated in accordance with the guidelines set by the International Council for Harmonization (ICH). This validation process ensures that the method is suitable for routine quality control analysis, making it convenient for regular use.

Vitis vinifera L. is a natural source of bioactive compounds that is already used for cosmeceutical and nutraceutical approaches. However, their phytochemical and antioxidant properties, although studied, have not been fully explored. We aimed to characterize V. vinifera L. cv. Falanghina seed extracts in different polarity solvents (hexane, ethyl acetate, ethanol, and a mixture of acetone–water) for their phytochemical contents, including the total phenolic compound content (TPC), free radical scavenging capacities, and antioxidant ability on HepG2 cells. We directly profiled the functional quality of V. vinifera seed extracts against H2O2-induced oxidative stress in HepG2 cells, focusing on mitochondrial functions. The content of bioactive compounds was characterized by LC-MS. To assess the cytocompatibility of the extracts, a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay was conducted. Results showed that extraction with ethyl acetate (18.12 mg GAE·g−1) and ethanol solvents (18.07 mg GAE·g−1), through Soxhlet, and with an acetone–water mixture (14.17 mg GAE·g−1), through maceration, yielded extracts rich in (poly)phenols, with good scavenging and antioxidant activity (98.32 I% for ethanol solvents and 96.31 I% for acetone–water mixture). The antioxidant effect of polyphenols is at least partially due to their capacity to maintain mitochondrial biogenesis and mitophagy, which elevates mitochondrial efficiency, resulting in diminished ROS production, hence re-establishing the mitochondrial quality control. These findings highlight the valorization of Vitis by-products to improve food functional characteristics.

Background: Sofosbuvir/ledipasvir (SOF/LDV), a combination of antiviral drugs, has been recently repurposed for COVID-19 management, according to Food and Drug Administration approval. Paracetamol (PAR) identified as a first-line antipyretic for COVID-19 symptoms' management. The use of these three drugs together has significantly influenced the management of COVID-19 by providing symptomatic relief via inhibiting viral activity. A validated ultra-high performance liquid chromatographic (UHPLC) method has been introduced for the quantification of these repurposed drugs in COVID-19 treatment. This novel chromatographic method allows the simultaneous detection of SOF, LDV, and PAR in bulk. Additionally, the method has been applied to determine the levels of SOF and LDV in human plasma samples with PAR used as an internal standard. Results: A new UHPLC method was developed, using a mobile phase with a combination of acetonitrile and 0.1% orthophosphoric acid in a proportion of 42:58 (v/v).Flow rate was set at 0.4 ml/min, and UV detection was adjusted at 254 nm. The concentration of SOF, LDV, and PAR were measured by their corresponding peak areas, and showed linear relationships between concentration and peak area within the ranges of (5–60) µg/ml for SOF, (2–22) µg/ml for LDV, and (1–22) µg/ml for PAR. The presented UHPLC method was used to quantify the amounts of SOF, LDV, and PAR in both bulk samples and human plasma samples being spiked with the mentioned analytes. The elution process was completed within 4 min, with retention times of 3.28 min for SOF, 2.28 min for LDV, and 1.70 min for PAR. The method showed high separation selectivity, with an injection volume of 1µl. The precision, accuracy and repeatability of the method were found to be within acceptable limits. Conclusion: The recently developed method has been successfully validated in accordance with the guidelines set by the International Council for Harmonization (ICH). This validation process ensures that the method is suitable for routine quality control analysis, making it convenient for regular use. [ABSTRACT FROM AUTHOR]

Eclipta prostrata L. (EPL), a medicinal plant, is widely utilized in the central highlands of Vietnam. This study aims to assess the chemical profile and potential medical effects of an EPL extract rich in flavonoids. A total of 36 secondary metabolites were identified from the EPL extract through GC-MS and UHPLC-UV analysis. Among them, 15 volatile compounds and several phenolic and flavonoid chemicals, including salicylic acid, epicatechin gallate, isovitexin, and apigetrin, were reported in EPL extract for the first time. This herbal extract demonstrated moderate inhibition against α-amylase and α-glucosidase, and high anti-oxidant and anti-acetylcholinesterase activities (IC50 = 76.8 ± 0.8 μg/mL). These promising attributes can be likely attributed to the high levels of major compounds, including wedelolactone (1), chlorogenic acid (3), epicatechin gallate (6), salicylic acid (8), isovitexin (9), apigetrin (11), and myricetin (12). These findings align with the traditional use of EPL for enhancing memory and cognitive function, as well as its potential benefits in diabetes management. The results of the molecular docking study reveal that the major identified compounds (1, 6, 9, and 11) showed a more effective acetylcholinesterase inhibitory effect than berberine chloride, with good binding energy (DS values, −12.3 to −14.3 kcal/mol) and acceptable values of RMSD (1.02–1.67 Å). Additionally, almost all the identified major compounds exhibited good ADMET properties within the required limits. [ABSTRACT FROM AUTHOR]

Purslane (Portulaca oleracea L., Portulacaceae) is a widespread edible plant with significant ethnobotanical and ethnopharmacological importance. The plant is characteristic for the presence of a class of indoline amide glucoside alkaloids, called cyclo-dopa amides, or oleraceins. Additionally, a new, structurally similar to oleraceins, class of indole amides have been discovered recently, called oleraindoles. These compounds have been evaluated to possess antiinflammatory and anticholinesterase activities. Herein, utilizing UHPLC-Orbitrap-MS with MS² filtering by diagnostic ion filtering (DIF), and diagnostic difference filtering (DDF) using different data analysis tools, eight compounds with oleraindole structure were tentatively identified. [ABSTRACT FROM AUTHOR]

Background: Fosfomycin acts against aerobic Gram−/+ bacteria by blocking the synthesis of peptidoglycan. Its use has been currently re-evaluated for intravenous administration for the treatment of systemic infections by multidrug-resistant bacteria. Concentration-/time-dependent activity has been suggested, with potential clinical advantages from prolonged or continuous infusion. Nevertheless, little is known about Fosfomycin stability in elastomeric pumps. The aim of the present work was stability investigation before administration at 4 °C and during administration at 34 °C. Methods: InfectoFos® (InfectoPharm s.r.l., Milan, Italy) preparation for intravenous use in elastomeric pumps at 4 °C and 34 °C was analyzed following EMA guidelines for drug stability. Samples were analyzed with an ultra-high performance liquid chromatography coupled with tandem mass spectrometry method on a LX50® UHPLC system equipped with a QSight 220® (Perkin Elmer, Milan, Italy) tandem mass spectrometer. Results: Fosfomycin in elastomeric preparation is stable for at least 5 days at a storage temperature of 4 °C and 34 °C. Conclusions: The results suggest Fosfomycin eligibility for continuous infusion even in the context of outpatient parenteral antibiotic therapy. Therefore, this approach should be tested in clinical and pharmacokinetic studies, in order to evaluate the possible gains in the pharmacokinetic profile and the clinical effectiveness. [ABSTRACT FROM AUTHOR]

Polycyclic aromatic hydrocarbons (PAHs) are widespread environmental contaminants formed during incomplete combustion or pyrolysis of organic material. The reliable quantification of PAH in airborne samples is still difficult, costly, and time-consuming due to the use of offline techniques, including long sampling on filters/adsorbents, laboratory extraction, purification, and concentration steps before analysis. To tackle these drawbacks, this work focused on the development of a fully automatic gas chromatograph (GC) equipped with a flame ionization detector (FID) and a sample preconcentration unit (PC) for gas sampling. This instrument was validated under laboratory-controlled conditions in the range 0–10 ng for 18 PAH. The chromatographic separation was rather satisfactory except for two PAH pairs, which were quantified together. For all compounds, the peak areas increased perfectly with the gaseous PAH concentration (R2 > 0.98), without any significant memory effect between two consecutive analyses. Considering a gaseous sample volume of 1 L, the extrapolated limits of detections (LOD) were in the range 19.9–62.6 ng/m3, depending on the PAH. Its analytical performances were then compared to those of the offline reference UHPLC-fluorescence method, widely used for airborne PAH monitoring. This was also compared with the very few portable or continuously operating instruments. [ABSTRACT FROM AUTHOR]

Cyanotis arachnoidea C. B. Clarke is a traditional Chinese medicinal herb that has a limited clinical use in the treatment of diabetes mellitus (DM) in minority areas of Guizhou in China. However, few prior reports are available on the quality control of Cyanotis arachnoidea, and its quality markers and hypoglycemic mechanism are still unclear. The purpose of this study is to explore the quality markers (Q-markers) of Cyanotis arachnoidea and predict its hypoglycemic mechanism. In this study, ultrahigh-performance liquid chromatography (UHPLC) fingerprint combined with chemical pattern recognition were performed, and four differential components were screened out as quality markers, including 20-Hydroxyecdysone, 3-O-acetyl-20-hydroxyecdysone, Ajugasterone C, and 2-O-acetyl-20-hydroxyecdysone. Network pharmacology analysis revealed 107 therapeutic target genes of Cyanotis arachnoidea in DM treatment, and the key targets were Akt1, TNF, IL-6, MAPK3, and JUN. The hypoglycemic mode of action of Cyanotis arachnoidea may be mediated by tumor necrosis factor (TNF) signaling, cancer, insulin resistance, and JAK-STAT pathways. Molecular docking analysis disclosed that the foregoing quality markers effectively bound their key target genes. An in vitro experiment conducted on pancreatic islet ß-cells indicated that the forenamed active components of Cyanotis arachnoidea had hypoglycemic efficacy by promoting PI3K/Akt and inhibiting MAPK signaling. UHPLC also accurately quantified the quality markers. The identification and analysis of quality markers for Cyanotis arachnoidea is expected to provide references for the establishment of a quality control evaluation system and clarify the material basis and hypoglycemic mechanisms of this traditional Chinese medicine (TCM). [ABSTRACT FROM AUTHOR]

People of Pakistan have undisturbed customs for the employment of medicinal plants for healthcare requisites. Chloroform extract of F. hygrometrica (CE FH) was examined for its ability to reduce inflammation and to produce analgesia. Carrageenan and formalin-induced paw edema model for inflammatory activity, hot-plate and tail-flick methods to assess analgesic activity were executed. Phytochemical analysis was done by UHPLC–MS and GC–mass spectrometer. The results demonstrated that in carrageenan-induced paw edema, maximum reduction in inflammation was observed at 5th hour at the dose 100 mg/kg; while at doses 250 and 500 mg/kg, maximum response was observed at 5th and 6th hours. Analgesic activity results indicated that maximum analgesia was observed up to 120 min at 100 mg/kg, while up to 90 min in case of 250 and 500 mg/kg doses. The formalin-induced rat paw edema showed significant (p < 0.05) anti-inflammatory activity after 5 days treatment. After, testing period of 10 days, the biochemical parameters such as CBC, CRP, serum enzymes like CAT, SOD, GSH and inflammatory mediators like TNF-α, IL-6, IL-4 and IL-10 were estimated. The administration of formalin resulted in an increase in the level of leucocytes, total WBC, CRP, serum enzymes and in the diameters of paw thickness, while pre-treatment with CE FH at dose levels of 100, 250 and 500 mg/kg exhibited a diminution in the levels of SOD, GSH, CAT, total RBC and HB. Acute inflammatory mediators such as TNFα, IL -6 and IL-4 were reduced, and IL-10 was upregulated in the treated group as compared to the control. Many phytoconstituents, i.e., chitobiose, chlorovulone III, γ-tocotrienol, emmotin, cassine, hexacosanedioic acid, neophytadiene, fumaric acid, neophytadiene, hexadecanoic acid, phytol and stigmasterol were detected during UHPLC–MS and GC–MS analysis seems to be responsible for the said activity in correlation with the already reported data about these compounds. The results concluded that CE FH possess noteworthy anti-inflammatory and central analgesic action at different doses (100, 250 and 500 mg/kg). [ABSTRACT FROM AUTHOR]

Sargassum hemiphyllum and Sargassum fusiforme are important benthic seaweeds that grow along the southeastern coast of China. The content of carotenoids in each population was detected by ultra-high performance liquid chromatography (UHPLC). The research results will enrich the theoretical basis and data support concerning the influencing factors of carotenoids in Sargassum. The inter-simple sequence repeat (ISSR) technique was used to study the genetic diversity of four S. hemiphyllum and two S. fusiforme populations, and the results provide a reference for the artificial cultivation of Sargassum. The total carotenoid content of Sargassum ranged from 161.79 ± 4.22 to 269.47 ± 6.15 μg/g. Among the carotenoids, β-carotene and fucoxanthin accounted for 80%, and levels in S. hemiphyllum were generally higher than those in S. fusiforme. The carotenoid contents of S. hemiphyllum from different areas were significantly different (P < 0.05), and the total carotenoids content decreased toward the southern region. The average heterozygosity H ranged from 0.29 to 0.49, and the Shannon diversity index I ranged from 0.44 to 0.69. The polymorphic loci, genetic diversity, and other indicators of S. hemiphyllum populations were higher than those of S. fusiforme, and the diversity of cultivated populations was not significantly lower. The results showed that the genetic variation of Sargassum is limited, and thus, more sexual reproduction can be attempted in breeding. Considering morphological indicators, genetic diversity indexes, and carotenoid content, S. hemiphyllum appears to have a higher commercial development value. [ABSTRACT FROM AUTHOR]

The goal of this study is to optimize a UAE method for the extraction of the main bioactive compounds present in the ginger rhizome (gingerols and shogaols). Ginger rhizome (Zingiber officinale) has a considerable content of bioactive compounds, in particular gingerols and shogaols, with interesting pharmacological activities such as anti-inflammatory, antioxidant, anti-cancer, and antimicrobial properties, among others. The isolation of these compounds requires an efficient extraction process with short extraction times and the employment of specific non-toxic solvents for humans. In this work, the optimization of an ultrasound-assisted extraction (UAE) method for the extraction of the main pungent compounds in the ginger rhizome, i.e., gingerols and shogaols, has been carried out. For this purpose, a Box–Behnken design (BBD) has been used to optimize the experimental design through a response surface methodology (RSM). The percentage of ethanol in the extraction solvent, the temperature, the amplitude, and the cycle of the ultrasounds, as well as the sample-to-solvent ratio, were the variables to be studied. Thus, the percentage of ethanol in the extraction solvent was identified as the most influential factor. Once the compounds were extracted, the identification of gingerols and shogaols was performed by ultra-high-performance liquid chromatography (UHPLC) coupled to a quadrupole-time-of-flight mass spectrometer (Q-ToF-MS), and the quantification by UHPLC coupled to a diode array detector (DAD) detector. Finally, the optimized UAE method required only 10 min of extraction time, presenting good repeatability and intermediate precision levels (<5%). The method was applied to extract gingerols and shogaols from diverse sources, thereby demonstrating its applicability and highlighting the potential variations in compound concentrations across different samples based on factors such as origin, and growing conditions, among others. [ABSTRACT FROM AUTHOR]