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This study aimed to determine the effectiveness of different green extraction techniques (GETs) on targeted bioactive compounds from artichoke leaf by-products using deep eutectic solvent extraction (DESE), supercritical CO2 extraction (SCO2E), subcritical water extraction (SWE), and ultrasound-assisted extraction (UAE). Moreover, (HR) LC-ESI-QTOF MS/MS and HPLC-PDA analyses were used to perform qualitative–quantitative analysis on the extracts, enabling the detection of several bioactive compounds, including luteolin, luteolin 7-O-glucoside, luteolin 7-O-rutinoside, apigenin rutinoside, chlorogenic acid, and cynaropicrin as the most representative ones. SWE showed better results than the other GETs (TPC: 23.39 ± 1.87 mg/g of dry plant, dp) and appeared to be the best choice. Regarding UAE, the highest total phenols content (TPC) was obtained with 50:50% v/v ethanol: water (7.22 ± 0.58 mg/g dp). The DES obtained with choline chloride:levulinic acid showed the highest TPC (9.69 ± 0.87 mg/g dp). Meanwhile, SCO2E was a selective technique for the recovery of cynaropicrin (48.33 ± 2.42 mg/g dp). Furthermore, the study examined the antioxidant activity (1.10–8.82 mmol Fe2+/g dp and 3.37–31.12 mmol TEAC/g dp for DPPH• and FRAP, respectively) and total phenols content via Folin–Ciocalteu's assay (198.32–1433.32 mg GAE/g dp), of which the highest values were detected in the SWE extracts. The relationship among the GETs, antioxidant assays, and compounds detected was evaluated using Principal Component Analysis (PCA). PCA confirmed the strong antioxidant activity of SWE and showed comparable extraction yields for the antioxidant compounds between UAE and DESE. Consequently, GETs selection and extraction parameters optimization can be employed to enrich artichoke leaf by-products' extracts with targeted bioactive compounds. [ABSTRACT FROM AUTHOR]

Obesity and hyperlipidemia have become major disorders predominantly causing prevailing cardiovascular diseases and ultimately death. The prolonged use of anti‐obesity drugs and statins for reducing obesity and blood lipid levels is leading toward adverse effects of kidneys and muscles, specifically rhabdomyolysis. The objective of this study is to evaluate potential of seeds of Ficus carica against hyperlipidemia. Various extracts and isolated compounds from fig seeds were analyzed and evaluated for their anti‐hyperlipidemic potential. Methanol extract and its ethyl acetate fraction showed maximum pancreatic lipase inhibition of 61.93% and 86.45% in comparison to reference drug Orlistat. Four compounds isolated by HPLC‐PDA technique were determined as Gallic acid, Catechin, Epicatechin, and Quercetin also showed strong potential to inhibit enzyme pancreatic lipase comparable to Orlistat. These isolated compounds were further analyzed for molecular docking and MM‐GBSA studies. Three ligands, namely Quercetin, Epicatechin, and Catechin were found more effective against pancreatic lipase as these possessed docking scores (−9.881, −9.741, −9.410) higher to that of the reference ligand Orlistat (−5.273). The binding free energies of these compounds were −55.03, −56.54, and 60.35 kcal/mol, respectively. The results have shown that Quercetin has the highest binding affinity correlating with the highest inhibition of pancreatic lipase enzyme 1LPB. Hence, it is suggested that seeds of F. carica have promising anti‐hyperlipidemic potential and foremost in reducing obesity. Summary: Various extracts, fractions of methanol extract, and isolated compounds of seeds of Ficus carica, in combating hyperlipidemia, were evaluated utilizing in vitro anti‐lipase activity and computational analysis.All extracts, methanol fractions and compounds isolated through high‐performance liquid chromatographic technique (HPLC) exhibited anti‐hyperlipidemic potential comparable to reference Orlistat.Molecular docking and MM‐GBSA studies illustrated that isolated ligand Quercetin along with Epicatechin and Catechin strongly inhibit enzyme pancreatic lipase (1LPB) and displayed a high docking score in comparison to reference ligand.Quercetin amongst four isolated compounds could be more effective in treating hyperlipidemia and obesity as compared to reference Orlistat. Significance Statement: Ficus carica possess potential constituents with profound therapeutic and traditional uses due to which the whole plant is considered medicinally important. This study focuses on the anti‐hyperlipidemic potential of seeds of F. carica against pancreatic lipase by using computational and in vitro studies. The results of this study provides the evidence that Quercetin exhibits a potent anti‐hyperlipidemic effect by inhibiting pancreatic lipase and also possess a greater binding affinity for pancreatic protein 1LPB as compared to reference Orlistat. [ABSTRACT FROM AUTHOR]

Lilium lancifolium Thunb. is a herbal medicine that is widely used to treat inflammation and lung diseases. In this study, a simultaneous quantitative method was developed for the quality control of BLL using high-performance liquid chromatography coupled with a photodiode array detector (HPLC–PDA), and their antioxidant effects were evaluated. Eight regalosides (i.e., regaloside A, B, C, E, F, H, I, and K) were selected as marker substances and separated on a Gemini C18 reversed-phase analytical column by gradient elution with distilled water–acetonitrile mobile phase containing 0.1% (v/v) formic acid. The method was validated with respect to linearity, sensitivities (limit of detection (LOD) and limit of quantitation (LOQ)), accuracy, and precision. The antioxidant effects of the extract and each component were evaluated using the 2,2-diphenyl-1-picrylhydrazyl radical scavenging assay and 2-2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) assay. The coefficients of determination values used as indicators of linearity for all components were ≥0.9999. LOD and LOQ concentrations were 0.10–0.66 μg/mL and 0.29–2.01 μg/mL, respectively. The recovery was 95.39–103.925% (relative standard deviation; RSD ≤ 2.55%), and precision RSD was <2.78%. The HPLC–PDA method was applied to real samples, and all components were detected at 1.12–29.76 mg/freeze-dried g. The evaluation of antioxidant effects showed that regalosides C, E, and K exhibited significant antioxidant effects. Our knowledge will be appropriately utilized in raw material management and conducting clinical and non-clinical studies on L. lancifolium or herbal medicine prescriptions containing L. lancifolium. [ABSTRACT FROM AUTHOR]

Background and Objectives: Seliciclib (SEL) is the first selective, orally bioavailable potential drug containing cyclin-dependent kinase inhibitors. Preclinical studies showed antitumor activity in a broad range of human tumor xenografts, neurodegenerative diseases, renal dysfunctions, viral infections, and chronic inflammatory disorders. To support the pharmacokinetics and aid in therapeutic monitoring of SEL following its administration for therapy, an efficient analytical tool capable of quantifying the concentrations of SEL in blood plasma is needed. In the literature, there is no existing method for quantifying SEL in plasma samples. This study introduces the first HPLC method with a photodiode array (PDA) detector for the quantitation of SEL in plasma. Materials and Methods: The chromatographic resolution of SEL and linifanib as an internal standard (IS) was achieved on Zorbax Eclipse Plus C18 HPLC column (150 mm length × 4.6 mm internal diameter, 5 µm particle size), with a mobile phase composed of acetonitrile–ammonium acetate, pH 5 (50:50, v/v) at a flow rate of 1.0 mL min−1. Both SEL and IS were detected by PDA at 230 nm. The method was validated according to the ICH guidelines for bioanalytical method validation. Results: The method exhibited linearity in concentrations ranging from 50 to 1000 ng mL−1, with a limit of quantitation of 66.1 ng mL−1. All remaining validation parameters satisfied the ICH validation criteria. The environmental sustainability of the method was verified using three extensive tools. The proposed HPLC-PDA method was effectively utilized to study the pharmacokinetics of SEL in rats after a single oral administration of 25 mg/kg. Conclusions: The proposed method stands as a valuable tool for studying SELs for pharmacokinetics in humans. It aids in achieving the targeted therapeutic advantages and safety of treatment with SEL by optimizing the SEL dosage and dosing schedule. [ABSTRACT FROM AUTHOR]

Background/Objectives: Uterine sarcoma, a rare cancer originating in the smooth muscle of the uterus, exhibits high rates of recurrence and metastasis. It represents one of the most challenging types of cancer due to its chemorefractory nature, showing little response to conventional chemotherapy methods and displaying a relative survival rate of 30–40%. A potentially promising approach for treating uterine sarcoma involves combination therapy with paclitaxel (PAC), a microtubule-targeting agent, and seliciclib (SEL), a cyclin-dependent kinase inhibitor. SEL has been identified as a drug that can enhance the effectiveness of PAC through synergistic effects. To further refine this treatment strategy, an efficient analytical tool capable of simultaneously measuring the concentrations of PAC and SEL in blood plasma is needed. This tool would make it easier to study the pharmacokinetic interactions of potential drugs and assist in monitoring therapy when administering this combination treatment. Regrettably, a method meeting these specific requirements has not been documented in the existing literature. Methods: This article introduces the first HPLC technique employing a PDA detector to concurrently measure PAC and SEL levels in plasma. The methodology underwent validation in accordance with the ICH standards for validating bioanalytical methods. Results: The method exhibited linearity in the concentrations ranging from 0.8 to 100 µg mL−1 for both PAC and SEL. The limits of quantification were determined and found to be 1.34 and 1.25 µg mL−1 for PAC and SEL, respectively. All the other validation criteria conformed to the ICH validation standards. The HPLC-PDA method was successfully employed to quantify both PAC and SEL in plasma samples with a high level of reliability (in terms of accuracy and precision). The eco-friendliness of the approach was verified using three thorough assessments. This technique serves as a valuable asset in establishing the correct dosage and administration schedule for the combined treatment involving PAC and SEL, ensuring the desired therapeutic effects and safety in managing uterine sarcoma. Conclusions: The proposed HPLC-PDA method is the first reliable and eco-friendly method developed to simultaneously determine PAC and SEL in high-throughput plasma samples in clinical laboratories. [ABSTRACT FROM AUTHOR]

Background/Objectives: Bacterial resistance and virulence are challenges in treating bacterial infections, especially in Klebsiella pneumoniae. Plants of the Launaea Cass. genus are used traditionally to address a variety of diseases, including infections, but the potential bioactive compounds are unknown. Our goals were to verify the potential contribution of two major polyacetylene glycosides isolated from our previous study, (3S,6E,12E)-6,12-tetradecadiene-8,10-diyne-1-ol 3-O-β-D-glucopyranoside (1) and bidensyneoside A (syn. gymnasterkoreaside A) [(3R,8E)-3-hydroxy-8-decene-4,6-diyn-1-yl β-D-glucopyranoside] (2), to the anti-infective properties of Launaea capitata and to develop a dependable HPLC method for their quantification; Methods: On a panel of K. pneumoniae clinical isolates, the antibacterial action of 1, 2, and the methanol extract of the whole L. capitata plant were evaluated by broth microdilution assay, while their antibiofilm action was evaluated by the crystal violet assay. qRT-PCR investigated luxS, mrkA, wzm, and wbbm genes that encode biofilm formation and quorum sensing (QS). The antibacterial activity of 1 was revealed by employing mice infection. Chromatographic separation was conducted using isocratic elution on a Hypersil BDS C18 column using a photodiode array (PDA) detector; Results: Compound 1 showed antibacterial activity with MIC values of 16–128 µg/mL. It remarkably reduced strong and moderate biofilm-forming bacterial isolates from 84.21% to 42.1% compared with the extract (68.42%) and 2 (78.95%). Compound 1 also downregulated the QS genes, luxS, mrkA, wzm, and wbbm, and exhibited in vivo antibacterial action through the enhancement of the histological construction of the liver and spleen, decreased TNF-α immunoreaction, bacterial burden, and the inflammatory mediators IL-1β and IL-6. A successful HPLC-PDA approach was developed to separate the binary mixture of 1 and 2 in less than 10 min with high sensitivity, with detection limits down to 0.518 and 0.095 µg/mL for 1 and 2, respectively; Conclusions: Compound 1 exhibited remarkable antibacterial and antibiofilm properties and may contribute to the anti-infectious traditional uses of L. capitata, meriting further clinical studies and serving as a reliable quality control biomarker for the plant. [ABSTRACT FROM AUTHOR]

Green analytical chemistry (GAC) primary goal is to develop environmental and health-friendly analytical methods by reduction or replacement of hazardous substances from analytical procedures. In this research, the application of GAC to quantify five β-lactams antibiotics (cefuroxime sodium, cefaclor, ertapenem sodium, ampicillin sodium and sulbactam sodium) by high-performance liquid chromatography (HPLC) using photodiode arrays (PDA) detector was developed. To achieve this, ethanol was used as a green replacement for methanol and acetonitrile, common solvents in chromatographic procedures. Several chromatographic conditions were investigated to accomplish the optimal conditions. The method validation followed the ICH Q2 (R1) guideline, and the developed method was successfully applied for quantifying some pharmaceutical products. [ABSTRACT FROM AUTHOR]

Introduction: Organic molecules that bind to cannabinoid receptors are known as cannabinoids. These molecules possess pharmacological properties similar to those produced by Cannabis sativa L. High‐performance liquid chromatography (HPLC) and ultra‐performance liquid chromatography (UPLC, also known as ultra‐high‐performance liquid chromatography, UHPLC) have become the most widely used analytical tools for detection and quantification of phytocannabinoids in various matrices. HPLC and UPLC (or UHPLC) are usually coupled to an ultraviolet (UV), photodiode array (PDA), or mass spectrometric (MS) detector. Objective: To critically appraise the literature on the application of HPLC and UPLC (or UHPLC) methods for the analysis of phytocannabinoids published from January 2020 to December 2023. Methodology: An extensive literature search was conducted using Web of Science, PubMed, and Google Scholar and published materials including relevant books. In various combinations, using cannabinoid in all combinations, cannabis, hemp, hashish, C. sativa, marijuana, analysis, HPLC, UHPLC, UPLC, and quantitative, qualitative, and quality control were used as the keywords for the literature search. Results: Several HPLC‐ and UPLC (or UHPLC)‐based methods for the analysis of phytocannabinoids were reported. While simple HPLC‐UV or HPLC‐PDA‐based methods were common, the use of HPLC‐MS, HPLC‐MS/MS, UPLC (or UHPLC)‐PDA, UPLC (or UHPLC)‐MS, and UPLC (or UHPLC)‐MS/MS was also reported. Applications of mathematical and computational models for optimization of protocols were noted. Pre‐analyses included various environmentally friendly extraction protocols. Conclusion: During the last 4 years, HPLC and UPLC (or UHPLC) remained the main analytical tools for phytocannabinoid analysis in different matrices. HPLC and UPLC (or UHPLC) are versatile analytical tools for the analysis of phytocannabinoids. This review critically appraises the literature on the application of HPLC and UPLC (or UHPLC) methods for the analysis of phytocannabinoids published from January 2020 to December 2023. During this period, HPLC and UPLC (or UHPLC) remained the main analytical tools for phytocannabinoid analysis. Applications of mathematical and computational models for optimization of protocols were noted. Pre‐analyses included various environmentally friendly extraction protocols. [ABSTRACT FROM AUTHOR]

Yeokwisan (YWS) is an herbal medicine prescription consisting of six oriental herbal medicines, developed to treat reflux esophagitis. We focused on developing an analytical method capable of simultaneously quantifying 13 compounds in YWS samples using high-performance liquid chromatography–photodiode array detection (HPLC–PDA) and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) and exploring their antioxidant effects. All compounds examined in both analytical systems were chromatographically separated on a SunFireTM C18 (4.6 × 250 mm, 5 μm) column and an Acquity UPLC BEH C18 (2.1 × 100 mm, 1.7 μm) column using gradient elution of a water–acetonitrile mobile phase. Antioxidant effects were evaluated based on radical scavenging activity (DPPH and ABTS tests) and ferrous ion chelating activity. In two analytical methods, the coefficient of determination of the regression equation was ≥0.9965, the recovery range was 81.11–108.21% (relative standard deviation (RSD) ≤ 9.33%), and the precision was RSD ≤ 11.10%. Application of the optimized analysis conditions gave quantitative analysis results for YWS samples of 0.02–100.36 mg/g. Evaluation of the antioxidant effects revealed that baicalein and baicalin exhibit significant antioxidant activity, suggesting that they play an important role in the antioxidant effects of YWS. [ABSTRACT FROM AUTHOR]

Saffron (Crocus sativus) floral by-products are a source of phenolic compounds that can be recovered and used in the nutraceutical, pharmaceutical, or cosmetic industries. This study aimed to evaluate the phenolic compounds' extraction using green extraction techniques (GETs) in saffron floral by-products and to explore the influence of selected extraction techniques on the phytochemical composition of the extracts. Specifically, ultrasound-assisted extraction (UAE), subcritical water extraction (SWE), and deep eutectic solvents extraction (DESE) were used. Phenolic compounds were identified with (HR) LC-ESI-QTOF MS/MS analysis, and the quantitative analysis was performed with HPLC-PDA. Concerning the extraction techniques, UAE showed the highest amount for both anthocyanins and flavonoids with 50:50% v/v ethanol/water as solvent (93.43 ± 4.67 mg/g of dry plant, dp). Among SWE, extraction with 96% ethanol and t = 125 °C gave the best quantitative results. The 16 different solvent mixtures used for the DESE showed the highest amount of flavonoids (110.95 ± 5.55–73.25 ± 3.66 mg/g dp), while anthocyanins were better extracted with choline chloride:butane-1,4-diol (16.0 ± 0.80 mg/g dp). Consequently, GETs can be employed to extract the bioactive compounds from saffron floral by-products, implementing recycling and reduction of waste and fitting into the broader circular economy discussion. [ABSTRACT FROM AUTHOR]

The use of z-drugs has increased worldwide since its introduction. Although the prescribing patterns of hypnotics differ among countries, zolpidem is the most widely used z-drug in the world. Zolpidem may be involved in poisoning and deaths. A simple and fast HPLC-PDA method was developed and validated. Zolpidem and the internal standard chloramphenicol were extracted from plasma using a sonication-assisted dispersive liquid–liquid microextraction procedure. The method was validated including selectivity, linearity, precision, accuracy, and recovery. The calibration range (0.15–0.6 µg/mL) covers therapeutic and toxic levels of zolpidem in plasma. The limit of quantification was set at 0.15 µg/mL. Intra- and interday accuracy and precision values were lower than 15% at the concentration levels studied. Excellent recovery results were obtained for all concentrations. The proposed method was successfully applied to ten real postmortem plasma samples. In our series, multiple substances (alcohol and/or other drugs) were detected in most cases of death involving zolpidem. Our analytical method is suitable for routine toxicological analysis. [ABSTRACT FROM AUTHOR]

Olive oil, particularly monovarietal virgin olive oil (MVOO), has garnered significant attention due to its potential health benefits attributed to a rich composition of bioactive compounds. This study aimed to assess the composition of bioactive compounds and the antioxidant activity of monovarietal virgin olive oil (MVOO). Specifically, the objective was to investigate the protective effects of MVOO in alleviating the adverse effects induced by titanium dioxide nanoparticles (NPTiO2). Bioactive compounds in MVOO were analyzed using UV–visible spectrophotometry, along with High-Performance Liquid Chromatography with a Photodiode Array (HPLC–PDA) for a comprehensive assessment. Antioxidant activity in vitro was evaluated through 2,2-diphenyl-1-picrylhydrazyl (DDPH) assays and on rats in vivo. A total of twenty-four male Wistar albino rats were randomly divided into four groups: one served as the control (Control), and the three remaining groups were injected with NPTiO2. Among the NPTiO2-injected groups, one received no treatment (NPTiO2), while the other two (NPTiO2 + MVOO1 and NPTiO2 + MVOO2) were treated with different doses of MVOO (2 g/kg bw and 6 g/kg bw). Commencing 24 h after NPTiO2 injection, the treatment with MVOO began, and body weight was consistently recorded. After 6 weeks of dietary manipulation, the fasting animals were sacrificed, and evaluations of hematological parameters, biochemical parameters, and oxidative stress markers in the liver and kidney were conducted. Histological examinations were performed to confirm protective effects. The analysis revealed significant levels of bioactive compounds in MVOO, with a remarkable DDPH antioxidant activity of 87.70%. Additionally, HPLC–PDA revealed the presence of quercetin and cinnamic acid. NPTiO2 induced oxidative stress, evidenced by increased biochemical parameters and elevated malondialdehyde levels in the liver and kidney (by + 91.30% and + 89.47%, respectively). Furthermore, there was a notable decrease in both hepatic and renal glutathione concentrations (-42% and -60%, respectively) and a reduction in antioxidant enzyme activities (GPx: -54.64% and -85.31%, GST: -77.70% and -74.33%, CAT: -87.21% and -73.11% for hepatic and renal, respectively), compared to the control group. Hematological profiles showed a decline in red blood cells and hemoglobin (-32.02%). Treatment with MVOO exhibited a protective effect by effectively mitigating biochemical parameters and enhancing antioxidant enzyme activities in the NPTiO2 + MVOO1 and NPTiO2 + MVOO2 groups, compared to the NPTiO2 group. Histological findings confirmed the protective effects of MVOO on liver and kidney damage caused by NPTiO2. MVOO demonstrated a potent protective effect against NPTiO2-induced oxidative stress, attributed to its richness in bioactive compounds. [ABSTRACT FROM AUTHOR]

A new HPLC-PDA method was developed and validated for simultaneous determination of five phenolic compounds (trans-and cis- isomers of tiliroside, quercetin-3-O-β-D-glucoside, ellagic acid, kaempferol-3-O-β-D-glucoside and isorhamnetin-3-O-glucoside) in the leaves of Hippophae salicifolia D. Don. Of the five compounds, three (tiliroside, quercetin-3-O-β-D-glucoside and ellagic acid) were isolated and characterised by spectroscopy techniques. The developed HPLC method provided a selective, sensitive and rapid analysis with good linearity (r2> 0.999), accuracy and precision. Also, the leaves of H. salicifolia were extracted by three different extraction techniques viz. reflux, microwave and ultrasound. Methanolic extracts prepared by reflux method showed the highest content of all the five compounds. [ABSTRACT FROM AUTHOR]

A field experiment following good agricultural practices was laid out to study the dissipation of spirotetramat (90 g a.i. ha−1 and 180 g a.i. ha−1) and chlorpyrifos (400 g a.i. ha−1 and 800 g a.i. ha−1) on cabbage heads and soil. Samples were processed using quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for residue estimation of spirotetramat and chlorpyrifos, which were further detected using HPLC–PDA and GC-FPD respectively. The residues of spirotetramat on cabbage heads reached below detection limit (BDL) (< 0.05 mg kg−1) on 7th and 10th day and for chlorpyrifos, BDL (< 0.01 mg kg−1) was achieved on 10th and 15th day for X and 2X dose, respectively. On 20th day after second spray, residues in soil were found to be BDL for both the pesticides. Half-life of spirotetramat and chlorpyrifos was found to be 3 and 2 days, respectively while a safe pre-harvest interval (PHI) of 9 days for spirotetramat and 10 days for chlorpyrifos is suggested on cabbage. The dietary risk assessment studies for various age groups of Indian population, ascertained safety of treated cabbage heads for consumption, as current study revealed that hazard quotient (HQ) < 1 and theoretical maximum dietary intake (TMDI) < maximum permissible intake (MPI) for both the pesticides at respective PHI. [ABSTRACT FROM AUTHOR]

Lichen specific metabolites (LSMs) have interesting biological activities and quantitative variations may be present intraspecifically. For example, variations in medullary fumarprotocetraric acid (FA) and cortical usnic acid (UA) were observed in the lichen Cladonia foliacea, but the mechanism of variation is not well understood. The current study aimed to characterise the quantitative variation of FA and UA and to investigate the association between lichen metabolite content and ecological / biological variables. Fungal and algal trees were constructed using fungal (nrITS, RPB2) and algal (nrITS) loci, respectively. Using a chiral chromatographic method, the contents of (-)-UA were determined in 29 C. foliacea specimens and range from 6.88 to 34.27 mg/g dry wt. The FA contents were lower and varied from 1.44 to 9.87 mg/g dry wt. Although the fungal tree showed two well resolved clades, no significant differences of UA or FA contents were found between the two fungal clades. However, a significantly higher UA/FA ratio as well as a unique habitat were found to be associated with specimens which contained the alga Asterochloris lobophora than those specimens associated other Asterochloris algae. Taking all predictive variables into account (i.e. substrate type, elevation, collection season, photobiont identity), the multivariate data analysis indicated that photobiont identity explained most of the variance of LSM contents in C. foliacea. Thus future LSM biosynthetic studies should take the photobiont into consideration when dealing with intraspecific quantitative variation. [ABSTRACT FROM AUTHOR]

Seaweed, in particular, brown seaweed, has gained research interest in the past few years due to its distinctive phenolic profile that has a multitude of bioactive properties. In order to obtain the maximum extraction efficiency of brown seaweed phenolic compounds, Response Surface Methodology was utilized to optimize the ultrasound-assisted extraction (UAE) conditions such as the amplitude, time, solvent:solid ratio, and NaOH concentration. Under optimal conditions, UAE had a higher extraction efficiency of free and bound phenolic compounds compared to conventional extraction (stirred 16 h at 4 °C). This led to higher antioxidant activity in the seaweed extract obtained under UAE conditions. The profiling of phenolic compounds using LC-ESI-QTOF-MS/MS identified a total of 25 phenolics with more phenolics extracted from the free phenolic extraction compared to the bound phenolic extracts. Among them, peonidin 3-O-diglucodise-5-O-glucoside and hesperidin 5,7-O-diglucuronide are unique compounds that were identified in P. comosa, E. radiata and D. potatorum, which are not reported in plants. Overall, our findings provided optimal phenolic extraction from brown seaweed for research into employing brown seaweed as a functional food. [ABSTRACT FROM AUTHOR]

Bopyeo-tang (BPT) is composed of six medicinal herbs (Morus alba L., Rehmannia glutinosa (Gaertn.) DC., Panax ginseng C.A.Mey., Aster tataricus L.f., Astragalus propinquus Schischkin, and Schisandra chinensis (Turcz.) Baill.) and has been used for the treatment of lung diseases. This study focused on establishing an analytical method that can simultaneously quantify nine target compounds (i.e., hydroxymethylfurfural, mulberroside A, chlorogenic acid, calycosin-7-O-glucoside, 3,5-dicaffeoylquinic acid, quercetin, kaempferol, schizandrin, and gomisin A) from a BPT sample using high-performance liquid chromatography with a photodiode array detector (HPLC–PDA) and ultra-performance liquid chromatography with tandem mass spectrometry (UPLC–MS/MS). The separation of compounds in both analyses was performed on a C18 reversed-phase column using the gradient elution of water–acetonitrile as the mobile phase. In particular, the multiple reaction monitoring mode was applied for quick and accurate detection in UPLC–MS/MS analysis. As a result of analyzing the two methods, HPLC–PDA and UPLC–MS/MS, the coefficient of determination of the regression equation for each compound was ≥0.9952, and recovery was 85.99−106.40% (relative standard deviation (RSD) < 9.58%). Precision testing of the nine compounds was verified (RSD < 10.0%). The application of these analytical assays under optimized conditions for quantitative analysis of the BPT sample gave 0.01–4.70 mg/g. Therefore, these two assays could be used successfully to gather basic data for clinical research and the quality control of BPT. [ABSTRACT FROM AUTHOR]

A simple new, rapid, sensitive, and cost-effective HPLC–PDA method was developed and validated for the determination of tetracycline (TC), oxytetracycline (OTC), and ciprofloxacin (CIP) simultaneously. Chromatographic separations were carried out using a reversed-phase Shim-pack GIS C18 column (4.60 × 250.00 mm; 5.00 µm) at 30°C. Oxalic acid (0.05 M), acetonitrile, and methanol were used as mobile phase under gradient elution conditions at the flow rate of 1.50 mL min−1. Detection wavelength was set at 330 nm. An aliquot of 20.00 µL solution was injected, and three drugs were eluted within 7.39 ± 0.05 min. As per ICH guidelines linearity, recovery, accuracy, precision, selectivity, specificity, sensitivity, stability, column efficiency, system suitability, and robustness were determined for the validation of the proposed method. Calibration curves were linear over a studied concentration range of 8.00 µg mL−1 with a correlation coefficient (r) of 0.999 for all drugs. Relative standard deviation (RSD) for intra− and interday precision was found less than 2.87% and 3.22%, respectively, indicating the method to be reproducible. The proposed method has been suitably applied for the estimation of TC, OTC, and CIP in pharmaceutical formulation and milk samples collected from local market in Bangladesh. Among 15 milk samples analyzed, most of the cases (more than 50%) TC, OTC, and CIP were detected above maximum residue levels (MRLs) though no significant toxicological effect on the health of consumers in the study area was identified.

ABSTRACTDate palm (Phoenix dactylifera L.) is an important fruit of the Middle East and North Africa with a high content of phenolic compounds. This study applied ultrasonic-assisted and conventional methods to extract phenolic compounds from date flesh and seed. The efficacy of the extraction methods is compared in terms of quantity, content, and antioxidant capacity of phenolic compounds. The highest total phenolic content (TPC) was found in ultrasonic-assisted date seed samples extracted by ethanol (18.53 mg GAE/g). In contrast, the TPC content of conventionally extracted seed samples ranged from 1.30 to 14.46 mg GAE/g. The TPC and antioxidant capacity values of phenolic compounds extracted from date flesh samples were lower than those extracted from seed samples. Liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS/MS) was used to characterize phenolic compounds. A total of 47 different phenolic compounds were identified, including 21 phenolic acids, 21 flavonoids, and 5 other polyphenols. High-performance liquid chromatography equipped with a photodiode array detector (HPLC-PDA) was used to quantify the phenolic compounds in different date samples. The highest content was found in ultrasonic-assisted date seed samples extracted in methanol solvent. The extract also contained epicatechin (36.12 μg/g), coumaric acid (27.05 μg/g), p-hydroxybenzoic acid (21.03 μg/g), syringic acid (19.85 μg/g), and epicatechin gallate (11.67 μg/g). The results showed that ultrasonic-assisted extraction could significantly increase the quantities of functional components of the extracts obtained from fresh date fruit samples.

Background and Objectives: Seliciclib (SEL) is the first selective, orally bioavailable potential drug containing cyclin-dependent kinase inhibitors. Preclinical studies showed antitumor activity in a broad range of human tumor xenografts, neurodegenerative diseases, renal dysfunctions, viral infections, and chronic inflammatory disorders. To support the pharmacokinetics and aid in therapeutic monitoring of SEL following its administration for therapy, an efficient analytical tool capable of quantifying the concentrations of SEL in blood plasma is needed. In the literature, there is no existing method for quantifying SEL in plasma samples. This study introduces the first HPLC method with a photodiode array (PDA) detector for the quantitation of SEL in plasma. Materials and Methods: The chromatographic resolution of SEL and linifanib as an internal standard (IS) was achieved on Zorbax Eclipse Plus C18 HPLC column (150 mm length × 4.6 mm internal diameter, 5 µm particle size), with a mobile phase composed of acetonitrile–ammonium acetate, pH 5 (50:50, v/v) at a flow rate of 1.0 mL min−1. Both SEL and IS were detected by PDA at 230 nm. The method was validated according to the ICH guidelines for bioanalytical method validation. Results: The method exhibited linearity in concentrations ranging from 50 to 1000 ng mL−1, with a limit of quantitation of 66.1 ng mL−1. All remaining validation parameters satisfied the ICH validation criteria. The environmental sustainability of the method was verified using three extensive tools. The proposed HPLC-PDA method was effectively utilized to study the pharmacokinetics of SEL in rats after a single oral administration of 25 mg/kg. Conclusions: The proposed method stands as a valuable tool for studying SELs for pharmacokinetics in humans. It aids in achieving the targeted therapeutic advantages and safety of treatment with SEL by optimizing the SEL dosage and dosing schedule.

This study aimed to determine the effectiveness of different green extraction techniques (GETs) on targeted bioactive compounds from artichoke leaf by-products using deep eutectic solvent extraction (DESE), supercritical CO2 extraction (SCO2E), subcritical water extraction (SWE), and ultrasound-assisted extraction (UAE). Moreover, (HR) LC-ESI-QTOF MS/MS and HPLC-PDA analyses were used to perform qualitative–quantitative analysis on the extracts, enabling the detection of several bioactive compounds, including luteolin, luteolin 7-O-glucoside, luteolin 7-O-rutinoside, apigenin rutinoside, chlorogenic acid, and cynaropicrin as the most representative ones. SWE showed better results than the other GETs (TPC: 23.39 ± 1.87 mg/g of dry plant, dp) and appeared to be the best choice. Regarding UAE, the highest total phenols content (TPC) was obtained with 50:50% v/v ethanol: water (7.22 ± 0.58 mg/g dp). The DES obtained with choline chloride:levulinic acid showed the highest TPC (9.69 ± 0.87 mg/g dp). Meanwhile, SCO2E was a selective technique for the recovery of cynaropicrin (48.33 ± 2.42 mg/g dp). Furthermore, the study examined the antioxidant activity (1.10–8.82 mmol Fe2+/g dp and 3.37–31.12 mmol TEAC/g dp for DPPH• and FRAP, respectively) and total phenols content via Folin–Ciocalteu’s assay (198.32–1433.32 mg GAE/g dp), of which the highest values were detected in the SWE extracts. The relationship among the GETs, antioxidant assays, and compounds detected was evaluated using Principal Component Analysis (PCA). PCA confirmed the strong antioxidant activity of SWE and showed comparable extraction yields for the antioxidant compounds between UAE and DESE. Consequently, GETs selection and extraction parameters optimization can be employed to enrich artichoke leaf by-products’ extracts with targeted bioactive compounds.

Lilium lancifolium Thunb. is a herbal medicine that is widely used to treat inflammation and lung diseases. In this study, a simultaneous quantitative method was developed for the quality control of BLL using high-performance liquid chromatography coupled with a photodiode array detector (HPLC–PDA), and their antioxidant effects were evaluated. Eight regalosides (i.e., regaloside A, B, C, E, F, H, I, and K) were selected as marker substances and separated on a Gemini C18 reversed-phase analytical column by gradient elution with distilled water–acetonitrile mobile phase containing 0.1% (v/v) formic acid. The method was validated with respect to linearity, sensitivities (limit of detection (LOD) and limit of quantitation (LOQ)), accuracy, and precision. The antioxidant effects of the extract and each component were evaluated using the 2,2-diphenyl-1-picrylhydrazyl radical scavenging assay and 2-2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) assay. The coefficients of determination values used as indicators of linearity for all components were ≥0.9999. LOD and LOQ concentrations were 0.10–0.66 μg/mL and 0.29–2.01 μg/mL, respectively. The recovery was 95.39–103.925% (relative standard deviation; RSD ≤ 2.55%), and precision RSD was L. lancifolium or herbal medicine prescriptions containing L. lancifolium.

Background/Objectives: Uterine sarcoma, a rare cancer originating in the smooth muscle of the uterus, exhibits high rates of recurrence and metastasis. It represents one of the most challenging types of cancer due to its chemorefractory nature, showing little response to conventional chemotherapy methods and displaying a relative survival rate of 30–40%. A potentially promising approach for treating uterine sarcoma involves combination therapy with paclitaxel (PAC), a microtubule-targeting agent, and seliciclib (SEL), a cyclin-dependent kinase inhibitor. SEL has been identified as a drug that can enhance the effectiveness of PAC through synergistic effects. To further refine this treatment strategy, an efficient analytical tool capable of simultaneously measuring the concentrations of PAC and SEL in blood plasma is needed. This tool would make it easier to study the pharmacokinetic interactions of potential drugs and assist in monitoring therapy when administering this combination treatment. Regrettably, a method meeting these specific requirements has not been documented in the existing literature. Methods: This article introduces the first HPLC technique employing a PDA detector to concurrently measure PAC and SEL levels in plasma. The methodology underwent validation in accordance with the ICH standards for validating bioanalytical methods. Results: The method exhibited linearity in the concentrations ranging from 0.8 to 100 µg mL−1 for both PAC and SEL. The limits of quantification were determined and found to be 1.34 and 1.25 µg mL−1 for PAC and SEL, respectively. All the other validation criteria conformed to the ICH validation standards. The HPLC-PDA method was successfully employed to quantify both PAC and SEL in plasma samples with a high level of reliability (in terms of accuracy and precision). The eco-friendliness of the approach was verified using three thorough assessments. This technique serves as a valuable asset in establishing the correct dosage and administration schedule for the combined treatment involving PAC and SEL, ensuring the desired therapeutic effects and safety in managing uterine sarcoma. Conclusions: The proposed HPLC-PDA method is the first reliable and eco-friendly method developed to simultaneously determine PAC and SEL in high-throughput plasma samples in clinical laboratories.

Background/Objectives: Bacterial resistance and virulence are challenges in treating bacterial infections, especially in Klebsiella pneumoniae. Plants of the Launaea Cass. genus are used traditionally to address a variety of diseases, including infections, but the potential bioactive compounds are unknown. Our goals were to verify the potential contribution of two major polyacetylene glycosides isolated from our previous study, (3S,6E,12E)-6,12-tetradecadiene-8,10-diyne-1-ol 3-O-β-D-glucopyranoside (1) and bidensyneoside A (syn. gymnasterkoreaside A) [(3R,8E)-3-hydroxy-8-decene-4,6-diyn-1-yl β-D-glucopyranoside] (2), to the anti-infective properties of Launaea capitata and to develop a dependable HPLC method for their quantification; Methods: On a panel of K. pneumoniae clinical isolates, the antibacterial action of 1, 2, and the methanol extract of the whole L. capitata plant were evaluated by broth microdilution assay, while their antibiofilm action was evaluated by the crystal violet assay. qRT-PCR investigated luxS, mrkA, wzm, and wbbm genes that encode biofilm formation and quorum sensing (QS). The antibacterial activity of 1 was revealed by employing mice infection. Chromatographic separation was conducted using isocratic elution on a Hypersil BDS C18 column using a photodiode array (PDA) detector; Results: Compound 1 showed antibacterial activity with MIC values of 16–128 µg/mL. It remarkably reduced strong and moderate biofilm-forming bacterial isolates from 84.21% to 42.1% compared with the extract (68.42%) and 2 (78.95%). Compound 1 also downregulated the QS genes, luxS, mrkA, wzm, and wbbm, and exhibited in vivo antibacterial action through the enhancement of the histological construction of the liver and spleen, decreased TNF-α immunoreaction, bacterial burden, and the inflammatory mediators IL-1β and IL-6. A successful HPLC-PDA approach was developed to separate the binary mixture of 1 and 2 in less than 10 min with high sensitivity, with detection limits down to 0.518 and 0.095 µg/mL for 1 and 2, respectively; Conclusions: Compound 1 exhibited remarkable antibacterial and antibiofilm properties and may contribute to the anti-infectious traditional uses of L. capitata, meriting further clinical studies and serving as a reliable quality control biomarker for the plant.

This study involved the development of an in-pipette tip solid-phase microextraction (SPME) method using activated charcoal as an adsorbent. Simultaneous determination of three sulphonamide antibiotic residues in environmental water was performed using this method, coupled with high-performance liquid chromatography-photodiode array (HPLC-PDA) detection. Seven extraction parameters were optimised by one-variable-at-a-time (OVAT) and response surface (RSM) methods. Optimum extraction efficiency was achieved when 10 mL of sample solution at a natural pH (pH 5–6) was loaded through a 1 mL pipette tip packed with 10 mg of adsorbent, washed with 1 mL of hexane and eluted with 500 µL of 1% ammonium in methanol solution. Under the optimised experimental condition, this method manifested good linearity (5–500 µg L−1) at the coefficient of determination, R2 of 0.9992 to 0.9993, high sensitivity (limit of detection, LOD: 0.38–1.14 µg L−1; limit of quantification, LOQ: 1.14–3.35 µg L−1), and satisfactory recoveries (82.8–108.7%) with acceptable reproducibility (RSD < 4.6%). Real sample analysis of five environmental water samples sourced from Universiti Malaya, Kuala Lumpur and Malacca showed that the samples contained either none or traces of the target sulphonamides (SAs) with their concentration lower than the LOQs. In contrast to other methods, the comparison outcomes depicted that this in-tip SPME method was beneficial in terms of its simple, reusable, cost-saving setup together with a significant reduction in chemical consumption. [ABSTRACT FROM AUTHOR]

Butternut squash (Cucurbita moschata) is recognized as a functional food due to its abundant content of health-promoting compounds, including carotenoids and polyphenols. The aim of this study was to examine the impact of industrial freezing stages on the bioaccessibility of carotenoids and polyphenols in organic Butternut squash supplied for baby food. Identification and quantification of bioactive compounds were carried out using UPLC-ESI-MS/MS and HPLC-PDA, respectively. The results revealed that industrial freezing of squash did not cause a significant change in bioaccessibility of α- and β-carotene. On the other hand, frozen squash was found to contain higher levels of bioaccessible epicatechin (main flavonoid) (117.5 mg/kg) and syringic acid (main phenolic acid) (32.0 mg/kg) compared to fresh internal fruit. Moreover, the levels of bioaccessible epicatechin and syringic acid were found to be the highest in discarded pomace and seed sample (454.0 and 132.4 mg/kg, respectively). Overall, this study emphasized that industrial freezing could be an effective strategy for preserving carotenoid bioaccessibility in organic Butternut squash, while also enhancing the levels of bioaccessible polyphenols. In addition, we also demonstrated that pomace and seed, which are discarded as waste, have significant potential to be utilized as a food source rich in bioactive compounds. [ABSTRACT FROM AUTHOR]

Phenolic compounds in agricultural raw materials can vary within a species and can be affected by a combination of such factors as growing region, weather conditions and fruit ripeness. Climatic differences between the southern, central and northern parts of Europe can cause differences in the phenolic compounds present in the plant. The research was aimed to investigate the phenolic compounds of berries of Sambucus nigra varieties grown for commercial production in Latvia. During the study four elderberry varieties were analysed - 'Haidegg 17', 'Korsör', 'Haschberg' and 'Emma'. All samples were analysed for total phenolic compound content (TPC), DPPH free radical scavenging activity and individual phenolic compounds. In addition, sample pH and total soluble solids (TSS) were measured. Results showed that 'Emma' berry samples had the highest value of TSS content - 10.5% (°Bx) and the lowest pH value - 3.65. The variety 'Korsör' showed the lowest TSS content - 8.1% (°Bx) as well as the lowest TPC and DPPH free radical scavenging activity, the variety 'Haschberg' showed the highest pH value. The variety 'Haidegg 17' stood out with a high TPC. In total six phenolic compounds were identified and quantified in the analysed samples - gallic acid, catechin, chlorogenic acid, p-coumaric acid, sinapic acid and 3,5-dihydroxybenzoic acid. According to the obtained results, it was evident that the indicators for some parameters differ from the information available in the literature about the composition of berries of crops grown in other regions. This suggests that it is worth further researching elder tree varieties grown in northern climate. [ABSTRACT FROM AUTHOR]

Drynariae Rhizoma (DR) is a functional food and traditional medicine that has been widely used for bone and joint disorders for thousands of years. In this study, 14 compounds were isolated from DR, and their structures were identified using UPLC/QTOF–MS, UPLC–ESI/LTQ–Orbitrap–HRMS, and 2D NMR and compared with those obtained in previous studies. An HPLC–PDA multi-component simultaneous quantitative determination method was developed for 12 of the 14 DR-derived compounds, excluding compounds with a content <1.5 mg. The developed HPLC method was validated based on linearity (r2 ≥ 0.999), limit of detection (0.01–0.65 μg/mL), limit of quantification (0.04–1.97 μg/mL), intra-day precision and accuracy ranges (0.06–2.85% and 95.03–104.75%, respectively), and inter-day precision and accuracy ranges (0.24–2.83% and 95.75–105.75%, respectively). The developed analysis method improved the resolution of compounds 4 and 5. In addition, this is the first quantitative analysis of compounds 7, 8, and 11 and the first simultaneous quantitative analysis of 12 compounds, including compounds 4, 7, 8, 10, 11, and 14. This study developed a rapid, accurate, and economical HPLC method for performing the simultaneous quantitative analysis of 12 secondary metabolites isolated from DR. [ABSTRACT FROM AUTHOR]

A tandem-column liquid chromatographic method was developed to separate ten non-steroidal anti-inflammatory drugs (Aceclofenac, Aspirin, Carprofen, Celecoxib, Diclofenac, Flurbiprofen, Ibuprofen, Ketoprofen, Naproxen, Salicylic Acid) using an achiral tandem-column configuration under reversed-phase conditions. An NSAID test mix was prepared with 0.5 mg/mL thiourea as a t0 marker and 0.5 mg/mL of the above NSAIDs in 1:1 acetonitrile: 0.2% formic acid. Three different 5-cm columns were investigated individually and in two different tandem-column configurations: an octyl (C8) column, a perfluorophenyl (PFP) column, and a biphenyl (BP) column. The two tandem configurations investigated were a PFP column followed by either a BP or C8 column. While none of the individual columns provided the selectivity needed to separate two sets of critical pairs (Ketoprofen and Naproxen; Flurbiprofen and Ibuprofen), the unique selectivity provided by the two tandem-column combinations enabled both critical pairs to be separated. The PFP + BP tandem column combination was able to separate the 10 NSAIDs with baseline or greater resolution in less than 25 min. [ABSTRACT FROM AUTHOR]

To gain a deep insight and to obtain a superior understanding about guanosine-based pathway, this paper reports an innovative approach to study this critical subject. Firstly, after an exhaustive analysis of literature with a focus in legal medicine and extracellular vesicles, it was understood that a new method is inevitable to follow, determine, and quantify these analytes (Guanosine monophosphate - GMP, guanosine diphosphate - GDP, guanosine triphosphate - GTP, Guanosine, Neopterin, and tetrahydrobiopterin - BH4).Starting from a previously method, we implemented and validated a new HPLC-DAD method in gradient elution mode with these six target analytes fully resolved in 18 min. The HPLC-DAD method uses a stationary phase XTIMATE C18 (4.6 mm × 250 mm, 5 µm, Welch, Shanghai, China) and mobile phase's phosphate buffer (40 mM, pH 7) (A) and Acetonitrile (B). Good correlation goes from 0.05 to 10 µg/mL with a limit of detection equal to 0.02 µg/mL and a limit of quantification equal to 0.05 µg/mL (R2 ≥ 0.9824).Method was tested on human extracellular vesicles, isolated from different human parts, like urine, saliva and muscle, giving interesting results as different quantification of analytes depending on the sample matrix used. Interesting to underline is that saliva was the poorest source of these analytes, if compared with growth medium and urine.

Yeokwisan (YWS) is an herbal medicine prescription consisting of six oriental herbal medicines, developed to treat reflux esophagitis. We focused on developing an analytical method capable of simultaneously quantifying 13 compounds in YWS samples using high-performance liquid chromatography–photodiode array detection (HPLC–PDA) and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) and exploring their antioxidant effects. All compounds examined in both analytical systems were chromatographically separated on a SunFireTM C18 (4.6 × 250 mm, 5 μm) column and an Acquity UPLC BEH C18 (2.1 × 100 mm, 1.7 μm) column using gradient elution of a water–acetonitrile mobile phase. Antioxidant effects were evaluated based on radical scavenging activity (DPPH and ABTS tests) and ferrous ion chelating activity. In two analytical methods, the coefficient of determination of the regression equation was ≥0.9965, the recovery range was 81.11–108.21% (relative standard deviation (RSD) ≤ 9.33%), and the precision was RSD ≤ 11.10%. Application of the optimized analysis conditions gave quantitative analysis results for YWS samples of 0.02–100.36 mg/g. Evaluation of the antioxidant effects revealed that baicalein and baicalin exhibit significant antioxidant activity, suggesting that they play an important role in the antioxidant effects of YWS.

Saffron (Crocus sativus) floral by-products are a source of phenolic compounds that can be recovered and used in the nutraceutical, pharmaceutical, or cosmetic industries. This study aimed to evaluate the phenolic compounds’ extraction using green extraction techniques (GETs) in saffron floral by-products and to explore the influence of selected extraction techniques on the phytochemical composition of the extracts. Specifically, ultrasound-assisted extraction (UAE), subcritical water extraction (SWE), and deep eutectic solvents extraction (DESE) were used. Phenolic compounds were identified with (HR) LC-ESI-QTOF MS/MS analysis, and the quantitative analysis was performed with HPLC-PDA. Concerning the extraction techniques, UAE showed the highest amount for both anthocyanins and flavonoids with 50:50% v/v ethanol/water as solvent (93.43 ± 4.67 mg/g of dry plant, dp). Among SWE, extraction with 96% ethanol and t = 125 °C gave the best quantitative results. The 16 different solvent mixtures used for the DESE showed the highest amount of flavonoids (110.95 ± 5.55–73.25 ± 3.66 mg/g dp), while anthocyanins were better extracted with choline chloride:butane-1,4-diol (16.0 ± 0.80 mg/g dp). Consequently, GETs can be employed to extract the bioactive compounds from saffron floral by-products, implementing recycling and reduction of waste and fitting into the broader circular economy discussion.

In the present study, date seeds as the main by-product of Phoenix dactylifera L. fruit, were roasted and analyzed for its acrylamide (AA) content for the first time. For this purpose, a QuEChERS (quick, easy, cheap, effective, rugged, and safe) protocol combined with HPLC–PDA was established for determination of AA in various roasted date seed varieties including Sayer, Shahani, Mazafati and Kabkab which the last one was used in the optimization experiments. To optimize the QuEChERS technique, AA was firstly extracted using acetonitrile from aqueous extract with or without n-hexane as the primary cleaning approach. Then, the selection of sorbent combination (primary secondary amine (PSA), octadecylsilane (C18), SAX (strong ion exchange), florisil, aluminum oxide) was performed for further clean-up. The protocol including n-hexane along with acetonitrile and further purification with PSA/SAX/C18 resulted in a light yellow, clear and transparent extract with 94.2% extraction recovery and 5.93–7.27% method intra-day precision. Validated analytical method showed the LOD of 7.73 µg L−1 and LOQ of 25.76 µg L−1. The intra-day (2.43–5.05%) and inter-day precision of instrument (1.73–4.96%) were also satisfactory. Mean AA content in four varieties of roasted date seeds ranged from 83.6 to 218.2 µg kg−1. The melanoidins content and browning index of samples were determined as well, and the values of 3.16–3.75 g 100 g−1 and 112.6–131.2 were obtained, respectively. In general, this study introduced roasted date seed as a contributor of consumer exposure to AA which can be determined successfully using QuEChERS method combined with HPLC–PDA. [ABSTRACT FROM AUTHOR]

Objective: The anti-diabetic efficacy of Atractylodes lancea water extract was verified by identifying the major active compounds, and quality control standards for water extracts were established by simultaneous HPLC quantification analysis. Methods: Thirteen compounds were isolated from the butanol fraction by bioactivity-guided approach using open-column chromatography. The compounds were identified by NMR and ESI/LTQ-Orbitrap-HRMS. The anti-diabetic activity was evaluated with anti-glycation and α-glucosidase assay. The simultaneous quantification by nine compounds was conducted by HPLC-PDA. Results: In total, 13 compounds from the butanol fraction were isolated. The water extract showed greater inhibitory effects than the hexane extract. Compounds 1, 2, 3, 5, 8, 10, 11, 12, and 13 showed high or significant activity. HPLC simultaneous analysis for these compounds was developed and validated to establish quality control standards, and the content standards of each compound were established through quantitative evaluation. Conclusion: To our knowledge, this study is the first to identify the main components and antiglycation, α-glucosidase inhibitory activity of the water extract of A. lancea. This study scientifically and systematically established the quality control standards of traditional herbal medicine traditional herbal medicine through the development of a simultaneous HPLC quantitative analysis method and the establishment of content standards. It also demonstrates the potential of A. lancea water extract as a natural alternative treatment for diabetes. [ABSTRACT FROM AUTHOR]

In natural products, the content and quality of the marker components differ depending on the part, production area, collection period, and extraction method; therefore, a standardized analysis method is required to obtain consistent results. This study developed a simultaneous analysis method for three marker components (7-methoxylutolin-5-O-glucoseide, pilloin 5-O-β-d-glucopyranoside, rutarensin) isolated and purified from Wikstroemia ganpi (W. ganpi). Simultaneous analysis was performed using high-performance liquid chromatography with photodiode array detection (HPLC-PDA) method that was validated according to the International Council for Harmonisation (ICH) guidelines. The developed analytical method exhibited linearity (r2 > 0.999), detection limits (0.72–3.34 μg/mL), and quantification limits (2.19–10.22 μg/mL). The relative standard deviation (RSD) value of intra- and inter-day precisions was less than 1.68%, and analyte recoveries (93.42–117.55%; RSD < 1.86%) were validated according to the analytical procedures, and all parameters were within the allowable range. Quantitative analysis of the three marker components from W. ganpi MeOH extract (WGM) showed 7-methoxylutolin-5-O-glucoseide with the highest content (51.81 mg/g). The inhibitory effects of WGM on cytochrome P450 (CYP) substrate drugs were further investigated. The in vitro study revealed that WGM inhibited the CYP3A-mediated metabolism of buspirone and that 7-methoxylutolin-5-O-glucoseide and pilloin 5-O-β-d-glucopyranoside inhibited the metabolism of buspirone with IC50 values of 2.73 and 18.7 μM, respectively. However, a single oral dose of WGM did not have significant effects on the pharmacokinetics of buspirone in rats, suggesting that WGM cannot function as an inhibitor of CYP3A-mediated metabolism in vivo. [ABSTRACT FROM AUTHOR]

The use of z-drugs has increased worldwide since its introduction. Although the prescribing patterns of hypnotics differ among countries, zolpidem is the most widely used z-drug in the world. Zolpidem may be involved in poisoning and deaths. A simple and fast HPLC-PDA method was developed and validated. Zolpidem and the internal standard chloramphenicol were extracted from plasma using a sonication-assisted dispersive liquid–liquid microextraction procedure. The method was validated including selectivity, linearity, precision, accuracy, and recovery. The calibration range (0.15–0.6 µg/mL) covers therapeutic and toxic levels of zolpidem in plasma. The limit of quantification was set at 0.15 µg/mL. Intra- and interday accuracy and precision values were lower than 15% at the concentration levels studied. Excellent recovery results were obtained for all concentrations. The proposed method was successfully applied to ten real postmortem plasma samples. In our series, multiple substances (alcohol and/or other drugs) were detected in most cases of death involving zolpidem. Our analytical method is suitable for routine toxicological analysis.

Seaweed, in particular, brown seaweed, has gained research interest in the past few years due to its distinctive phenolic profile that has a multitude of bioactive properties. In order to obtain the maximum extraction efficiency of brown seaweed phenolic compounds, Response Surface Methodology was utilized to optimize the ultrasound-assisted extraction (UAE) conditions such as the amplitude, time, solvent:solid ratio, and NaOH concentration. Under optimal conditions, UAE had a higher extraction efficiency of free and bound phenolic compounds compared to conventional extraction (stirred 16 h at 4 °C). This led to higher antioxidant activity in the seaweed extract obtained under UAE conditions. The profiling of phenolic compounds using LC-ESI-QTOF-MS/MS identified a total of 25 phenolics with more phenolics extracted from the free phenolic extraction compared to the bound phenolic extracts. Among them, peonidin 3-O-diglucodise-5-O-glucoside and hesperidin 5,7-O-diglucuronide are unique compounds that were identified in P. comosa, E. radiata and D. potatorum, which are not reported in plants. Overall, our findings provided optimal phenolic extraction from brown seaweed for research into employing brown seaweed as a functional food.

Bopyeo-tang (BPT) is composed of six medicinal herbs (Morus alba L., Rehmannia glutinosa (Gaertn.) DC., Panax ginseng C.A.Mey., Aster tataricus L.f., Astragalus propinquus Schischkin, and Schisandra chinensis (Turcz.) Baill.) and has been used for the treatment of lung diseases. This study focused on establishing an analytical method that can simultaneously quantify nine target compounds (i.e., hydroxymethylfurfural, mulberroside A, chlorogenic acid, calycosin-7-O-glucoside, 3,5-dicaffeoylquinic acid, quercetin, kaempferol, schizandrin, and gomisin A) from a BPT sample using high-performance liquid chromatography with a photodiode array detector (HPLC–PDA) and ultra-performance liquid chromatography with tandem mass spectrometry (UPLC–MS/MS). The separation of compounds in both analyses was performed on a C18 reversed-phase column using the gradient elution of water–acetonitrile as the mobile phase. In particular, the multiple reaction monitoring mode was applied for quick and accurate detection in UPLC–MS/MS analysis. As a result of analyzing the two methods, HPLC–PDA and UPLC–MS/MS, the coefficient of determination of the regression equation for each compound was ≥0.9952, and recovery was 85.99−106.40% (relative standard deviation (RSD) < 9.58%). Precision testing of the nine compounds was verified (RSD < 10.0%). The application of these analytical assays under optimized conditions for quantitative analysis of the BPT sample gave 0.01–4.70 mg/g. Therefore, these two assays could be used successfully to gather basic data for clinical research and the quality control of BPT.

Objectives: Neurada procumbens L. (Neuradaceae) is a Cholistani desert plant traditionally employed in fever, inflammations, diabetes and hepatitis. The purpose of this study was to determine the chemical composition, anti-bacterial, antibiofilm and antioxidant activities of various extracts of this important medicinal plant; separately for its aerial and floral parts. Methods: The phytochemical screening (by HPLC analysis), antioxidant (by DPPH assay), antibacterial (by disc diffusion test and MIC) and anti-biofilm potential against seven bacterial strains (E. coli, K. pneumoniae, S. aureus, S. aureus MDR, P. aeruginosa, P. aeruginosa MDR and P. vulgaris) were determined by aqueous, methanol, n-butanol, ethyl acetate, n-hexane and dichloromethane extracts of floral and aerial parts of N. procumbens. Results: The floral MetOH and DCM extracts were found to contain higher polyphenolic contents including 2,3-di methoxy benzoic acid (38.21 µg/mg), chlorogenic acid (26.59 µg/mg) and catechin (14.24 µg/mg) and exhibited a comparatively higher antioxidant (IC50 13.5 mm zone of inhibition and MICs 62.5–125 µg/ml) against P. aeruginosa MDR and S. aureus in anti-bacterial activity. In an anti-biofilm assay, MetOH and DCM floral extracts showed a promising potential (>85 % biofilm inhibition) with IC50

Tanacetum parthenium, also known as feverfew, is rich in bioactive compounds, namely sesquiterpene lactones, flavonoids, and volatile oils. Sesquiterpene lactones possess anti-migraine activity, while phenolic compounds possess anti-inflammatory and antioxidant action. Phytochemical composition determines the pharmacological activity and so profiling is essential in quality assessment. The study aimed to evaluate cultivated feverfew plants' phenolic profiles and antioxidant activity. Eleven phenolic compounds were identified in the samples of feverfew in Ukraine. Hydroxycinnamic acids predominate in the quantitative content of all the samples, namely chlorogenic acid, 3,5-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid. The total content of flavonoids ranged from 0.8 to 2.6%; the content of hydroxycinnamic acids varied from 3.3 to 6.5%. The obtained data testify to the prospects of using Ukrainian feverfew as a raw material with a significant content of phenolic substances to develop new herbal medicines. [ABSTRACT FROM AUTHOR]

Anemarrhena asphodeloides Bunge (A. asphodeloides Bunge) root extract contains nyasol as its main ingredient. Nyasol was extracted and prepared as a cosmetic raw material in 95% ethanol. To identify nyasol as a marker compound qualitative analysis was performed using ultra-performance liquid chromatographyi coupled with electrospray ionization–tandem mass spectrometry. Below a nyasol content of 12 μg/mL, the root extract exhibited negligible cytotoxicity. In this concentration range, melanin production in B16F10 mouse melanoma cells decreased as the concentration of nyasol increased, indicating a skin-whitening effect. In addition, an antiwrinkling effect was confirmed by evaluating the inhibition of MMP-1 protein expression in TNF-α-treated HaCaT cells by either A. asphodeloides Bunge root extract (>0.31 μg/mL) or nyasol (>0.25 μg/mL). High-performance liquid chromatography-coupled with a photodiode detector array was used to show that our extract contained 5.06 ± 0.01% nyasol. Furthermore, when this analysis method was applied for the quality control of a cream product containing 2 wt.% of A. asphodeloides Bunge root extract, the measured content of nyasol (0.1%) was over 90% of the nominal quantity. Therefore, the product was deemed to be within the required quality standards. [ABSTRACT FROM AUTHOR]

Zingiber Officinale Roscoe, a famous plant that has been used worldwide for the consumption and treatment of human ailments. In Thailand, ginger is grown in many areas throughout the country. Lampang is subjected to be one of the northern provinces where ginger growing had remarkably increased in recent years. This study aimed to determine the amounts of 6-gingerol and camphene from Z. Officinale Roscoe grown in Ban Pha-Daeng, Ngao District, Lampang Province in 2020 and 2021. Dried rhizome of Z. Officinale was extracted with hexane, ethyl acetate and methanol. 6-gingerol and camphene of three crude extracts were analyzed using High Performance Liquid Chromatography –Photo Diode Array (HPLC-PDA) method. The content of 6-gingerol in all extracts was found in the range of 1.95 to 13.85 mg/g while the content of camphene was found in the range of 1.39 to 51.97 mg/g. The level of 6-gingerol and camphene in ethyl acetate extracts was greater than the hexane and methanol extracts. The result indicated the amounts of 6-gingerol and camphene of Z. Officinale grown in 2020 was higher compared to the content in 2021. [ABSTRACT FROM AUTHOR]

Organic colorants of textiles found in the female burial of Lieto Ristinpelto, SW Finland, were analyzed by HPLC-PDA. The textiles’ visible colors varied from different brownish shades to blueish, greenish, and reddish hues. The aim of the chromatographic analysis was to deepen the current understandings of the dyes used in Finland at the transition between the 12th and 13th centuries AD, i.e., at the beginning of the local Medieval period, and to contribute important new information about dyes and clothing from this less-known period of textile history of Finland. The textile finds consisted of a bronze spiral ornamented shawl, an apron tied at the waist, two tablet-woven bands, and a diagonally plaited band with plaited tassels. A unique find was a textile possibly made using the sprang technique. Other textile finds were an orange wool tabby and twill fragments. Analysis of thirty samples from fourteen different textiles indicated that woad colorants were present in most samples, accompanied with lichen compounds, and dyer’s madder was in two visually orange fragments. The visually reddish samples contained luteolin, but no red colorants.

Abstract Etoricoxib (ETO), Paracetamol (PCM), and two toxic impurities for Paracetamol impurity K (4-aminophenol (PAP)) and impurity E (para-hydroxy acetophenone (PHA)) were separated using a simple and selective HPLC method that was tested for the first time. PCM is a commonly used analgesic and antipyretic medication that has recently been incorporated into COVID-19 supportive treatment. Pharmaceuticals containing PCM in combination with other analgesic-antipyretic drugs like ETO help to improve patient compliance. The studied drugs and impurities were separated on a GL Sciences Inertsil ODS-3 (250 × 4.6) mm, 5.0 µm column, and linear gradient elution was performed using 50 mM potassium dihydrogen phosphate adjusted to pH 4.0 with ortho-phosphoric acid and acetonitrile as mobile phase at 2.0 mL/min flow rate at 25 °C and UV detection at 220 nm. The linearity range was 1.5–30.0 µg/mL for ETO and PCM while 0.5–10.0 µg/mL for PAP and PHA, with correlation coefficients (r) for ETO, PCM, PAP, and PHA of 0.9999, 0.9993, 0.9996, and 0.9998, respectively. The proposed method could be used well for routine analysis in quality control laboratory.

Brown seaweed is rich in phenolic compounds and has established health benefits. However, the phenolics present in Australian beach-cast seaweed are still unclear. This study investigated the effect of ultrasonication and conventional methodologies using four different solvents on free and bound phenolics of freeze-dried brown seaweed species obtained from the southeast Australian shoreline. The phenolic content and their antioxidant potential were determined using in vitro assays followed by identification and characterization by LC-ESI-QTOF-MS/MS and quantified by HPLC-PDA. The Cystophora sp. displayed high total phenolic content (TPC) and phlorotannin content (FDA) when extracted using 70% ethanol (ultrasonication method). Cystophora sp., also exhibited strong antioxidant potential in various assays, such as DPPH, ABTS, and FRAP in 70% acetone through ultrasonication. TAC is highly correlated to FRAP, ABTS, and RPA (p < 0.05) in both extraction methodologies. LC-ESI-QTOF-MS/MS analysis identified 94 and 104 compounds in ultrasound and conventional methodologies, respectively. HPLC-PDA quantification showed phenolic acids to be higher for samples extracted using the ultrasonication methodology. Our findings could facilitate the development of nutraceuticals, pharmaceuticals, and functional foods from beach-cast seaweed. [ABSTRACT FROM AUTHOR]

This study aimed to investigate the effect of four green extraction techniques (ultrasound-assisted extraction, UAE; supercritical fluid extraction, SFE; subcritical water extraction, SWE; and extraction using deep eutectic solvents, DES) on the extraction of targeted flavonoids from edible feijoa flowers. The bioactive components in the obtained extracts were quantified by High-Performance Liquid Chromatography—Photodiode Array Detector (HPLC-PDA). Moreover, total polyphenol content and antioxidant activity by DPPH•, ABTS•+, FRAP, and CUPRAC assays were investigated. UAE generally gave the highest yields for isoquercitrin and quercetin content (18.36–25.33 and 10.86–16.13 µg/g), while DES extraction with choline chloride:lactic acid (1:2) and H2O content of 50% gave the highest yield of chrysanthemin (90.81 µg/g). The highest yield of flavone (12.69 mg/g) was obtained with supercritical CO2 at 300 bar. Finally, UAE gave the highest total polyphenol content (ca. 64 mg GAE/g) and antioxidant activity at 70 °C during 30 min with 40% (0.84 mmol TEAC/g and 2.25 mmol Fe2+/g, for ABTS•+ and CUPRAC, respectively) and 60% ethanol-water solution (0.49 mmol TEAC/g and 2.09 mmol Fe2+/g, for DPPH• and FRAP, respectively). The eco-friendly extraction techniques resulted in selective methods capable of extracting targeted bioactive compounds from edible feijoa flowers. [ABSTRACT FROM AUTHOR]