Phenolic profiles of Australian monofloral Eucalyptus, Corymbia, Macadamia and Lophostemon honeys via HPLC-DAD analysis.

Australian honey samples from four botanical genera (Lophostemon, Eucalyptus, Macadamia and Corymbia) were investigated for their phenolic content. An improved phenolic extraction and high-performance liquid chromatography-diode array detection (HPLC-DAD) analysis method allowed for the rapid and reliable identification of phenolic compounds. A concentrated liquid-liquid extraction method with an acidified aqueous solution and acetonitrile was optimised to isolate phenolic compounds from the honey matrix. The concentrated extraction method improved sensitivity and permitted the identification of phenolics present at low concentrations (LOD: 0.012-0.25 mg/kg and LOQ: 0.040-2.99 mg/kg). The optimised HPLC-DAD chromatographic conditions gave stable retention times, improved peak separation and allowed for the inexpensive detection of each of the 109 phenolic compounds at their maximum absorbance wavelength. Out of the 109 phenolic compounds included in this study, 49 were identified in the Australian honeys tested. Furthermore, 25 of the 49 compounds were determined to be markers specific to honey floral origin.

Cyanide profiling in stone fruit syrups: A comparative study of distillation techniques, a novel derivatization method, and cyanide composition in Maesil (Prunus Mume) syrup.

Cyanide ion was derivatized with o-phthalaldehyde and 3-mercaptopropionic acid for high-performance liquid chromatography-diode array detector analysis. The structure was elucidated using nuclear magnetic resonance spectroscopy and ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry. Method validation was conducted for three distillation methods to analyze cyanogenic glycosides, cyanohydrins, and free cyanide in fruit syrup. Acid-aided distillation only detected free cyanide, while direct distillation detected both free cyanide and cyanohydrins, and enzyme-aided distillation reflected all three types. These approaches were applied to stone fruit syrups in South Korean markets and households. Among tested, maesil (Prunus mume) syrup contained the highest amount of total cyanide, reaching a maximum of 21.9 mg/kg (cyanide ion equivalent), compared to other syrups. Investigation of cyanide composition changes during maesil syrup production revealed that free cyanide occupies the lowest proportion. Cyanogenic glycosides degraded gradually during aging, while cyanohydrins remained the majority after 12 months aging.

Polycyclic aromatic hydrocarbons (PAHs) in black crusts on stone monuments in Milan: detection, quantification, distributions, and source assessment.

In the field of conservation of cultural heritage, one must always consider the environmental conditions in which the works of art are located and the level of atmospheric pollution to which they are exposed, especially in the case of monuments stored outdoors. The present study is focused on the detection and the quantification of polycyclic aromatic hydrocarbons (PAHs) in black crust samples from the Monumental Cemetery of Milan (Italy), and the assessment of their sources through the analysis of the distributions of the different compounds in the samples, together with the use of diagnostic ratios. Six black crust samples taken from funerary monuments were analyzed. Fourteen polycyclic aromatic hydrocarbons were identified (naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, chrysene, benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-cd]pyrene) by high-performance liquid chromatography with a diode-array detector (HPLC-DAD), with a total concentration from 0.72 to 3.81 µg/g (mean of 1.87 µg/g). The known carcinogenic benzo[a]pyrene accounted for 5-10% of the total polycyclic aromatic hydrocarbons in the samples analyzed, with concentrations up to 0.20 µg/g. Moreover, the study of the distribution and diagnostic ratios allowed us to confirm that anthropogenic sources such as traffic and the proximity of the train station are the major causes of the degradation of the monuments contained in this Cemetery.

Impact of traditional and innovative cooking techniques on Italian black rice (Oryza sativa L., Artemide cv) composition.

Due to its high polyphenol content, black rice plays a significant role in good nutrition; however, these antioxidant compounds are affected by heat treatments required for the rice consumption. The aim of this work was to investigate how cooking affects the composition of Artemide black rice, comparing innovative methods, such as sous vide, with traditional domestic techniques (risotto and pilaf). Proteins and ashes were not affected by cooking, except for pilaf rice, where a 42 % ashes decrease was observed; fiber content increased after all cooking methods, reaching a 29 % increase in the risotto. Antioxidant activity, total polyphenols, anthocyanins and proanthocyanidins were reduced on average of 40 %, 34 %, 43 % and 39 %, respectively. Individual anthocyanins decreased, while phenolic acids and other flavonoids presented different behaviours, also depending if considered in their free or bound form. Cyanidin-3-O-glucoside was reduced up to 56 % in the sous vide cooked rice at 99 °C, and only by 45 % and 37 % in the risotto and sous vide cooked rice at 89 °C, respectively. Traditional risotto preparation and the innovative sous vide cooking at 89 °C also maintained the highest antioxidant polyphenols content, saving 63 % of the antioxidant activity in respect to the raw black rice. Concluding, these last techniques can be suggested for a better preservation of bioactive compounds.

Phytochemical Profiling and Antimicrobial Properties of Various Sweet Potato (Ipomoea batatas L.) Leaves Assessed by RP-HPLC-DAD.

This study aimed to investigate the leaves of six cultivars of Ipomoea batatas L. from the USA, focusing on their Total Polyphenol Content (TPC), Total Flavonoid Content (TFC), antioxidant, and antimicrobial activities. TPC and TFC ranged from 7.29 ± 0.62 to 10.49 ± 1.04 mg TAE/g Dw, and from 2.30 ± 0.04 to 4.26 ± 0.23 mg QE/g Dw, respectively, with the highest values found in the 'O'Henry' variety. RP-High-Performance Liquid Chromatography identified six phenolic and flavonoid compounds: caffeic acid, chlorogenic acid, 3,5-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, and quercetin, excluding gallic acid. The highest levels of these compounds were found in acidified methanolic extracts. Antioxidant activities, measured by ABTS and DPPH assays, showed low IC50 values ranging from 94.6 ± 2.76 to 115.17 ± 7.65 µg/mL, and from 88.83 ± 1.94 to 147.6 ± 1.22 µg/mL. Ferric Ion-Reducing Antioxidant Potential (FRAP) measurements indicated significant antioxidant levels, varying from 1.98 ± 0.14 to 2.83 ± 0.07, with the 'O'Henry' variety exhibiting the highest levels. The antimicrobial activity test included five Gram-positive bacteria, three Gram-negative bacteria, and two pathogenic fungi. S. aureus, S. mutans, L. monocytogenes, E. coli, S. dysenteriae, and C. albicans were most susceptible to the methanolic extract. This study underscores the impressive antioxidant and antimicrobial activities of sweet potato leaves, often discarded, making them a valuable source of natural antioxidants, antimicrobials, and other health-promoting compounds.

Bar adsorptive microextraction and liquid chromatography-diode array detection of synthetic cannabinoids in oral fluid.

In recent years, synthetic cannabinoids (SCs) have become a major public health issue. For this reason, there is a need for innovative analytical methods that allow its monitoring in biological matrices. In this work, we propose a novel methodology to screen eight SCs (AM-694, cumyl-5F-PINACA, MAM-2201, 5F-UR-144, JWH-018, JWH-122, UR-144 and APINACA) in oral fluids. A bar adsorptive microextraction method followed by microliquid desorption combined with high-performance liquid chromatography with diode array detection (BAµE-µLD/HPLC-DAD) was developed to monitor the target SCs. The main factors affecting the BAµE technology were fully optimized for oral fluid analysis. Under optimized experimental conditions, the proposed methodology showed good linear dynamic ranges from 20.0 to 2000.0 µg L-1 (r2 > 0.99, relative residuals < 15%), limits of detection between 2.0 and 5.0 µg L-1 and suitable average recovery yields (87.9-100.5%) for the eight studied SCs. The intra- and interday accuracies (bias ≤ ± 14.7%) and precisions (RSD ≤ 14.9%) were also evaluated at three spiking levels. The validated methodology was then assayed to oral fluid samples collected from several volunteers. The proposed analytical approach showed remarkable performance and could be an effective alternative for routine monitoring of the target compounds in oral fluid.

HPLC-DAD method for simultaneous determination of gallic acid, catechins, and methylxanthines and its application in quantitative analysis and origin identification of green tea.

The high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD) was optimized for the simultaneous determination of 11 compounds, belonging to polyphenols (gallic acid and seven catechins) and methylxanthines (caffeine, theobromine, and theophylline). The results obtained for all the validation parameters of the HPLC-DAD method showed that the method is sensitive enough for routine analysis with basic chromatographic equipment, thus it has a significant potential to be highly applicable in common laboratory practice. The method was used in the analysis of 60 green tea infusions originating from four tea-producing countries. The dataset contributes to enhancing current data on green tea. The analysis of green tea extracts revealed significant differences depending on the origin of the samples. Linear Discriminant Analysis (LDA) was applied to test the accuracy of identification of the origin of the tea samples, based on the chemical composition of tea with a focus on polyphenolic compounds and methylxanthines analysed in this study. Based on cross-validation results, the model showed 93.75 % accuracy in the classification of green tea originating from Japan, China (Mainland), China (Taiwan) and South Korea.

Phytochemical, biochemical and physiological assessment of the protective effect of local Trigonella foenum graecum in rats administered a ß-cell toxicant.

This study sought to assess quantitatively individual and total polyphenols, mineral composition, antioxidant and antiglycation activity of Algerian fenugreek seeds (AFS) as well as the protective effect of its supplementation on streptozotocin (STZ)-induced diabetic rats via alleviation of oxidative stress, inflammation and histological disarray. Forty rats were partitioned into four groups (i) non-diabetic rats, (ii) non-diabetic rats+ 10% AFS, (iii) diabetic rats, (iv) diabetic rats +10% AFS. Flame-SAA analysis revealed a rich content in micro-elements, HPLC-DAD-LFD analysis revealed several components with rutin and ferulic acid being the major compounds in AFS hydro-methanolic extract while spectrophotometric assays scrutinized moderate contents in total phenolic and flavonoids. The extract was potent in scavenging ABTS•+, DPPH+, reducing Fe3+, Mo6+ and inhibiting AGEs. In vivo, 10%AFS- supplemented diet (w/w) was found to elicit a significant reduction in glycemia, TNF-α, IL-6, CRP, liver markers, lipid peroxidation (MDA) and protein carbonyl (PCO) along with improvement in reduced glutathione (GSH) amount, glutathione peroxidase (GPx), catalase (CAT) and glutathione-S-transferase (GST) activities with rejuvenation of hepatic and pancreatic micro-anatomical features. These outcomes disclosed that AFS is endowed with biologically effective components which could be decent applicant to attain the objective of glycation, oxidative stress and mitigating diabetes-related complications.

A sustainable HPLC method coupled with diode array detection for versatile quantification of telmisartan, chlorthalidone and amlodipine in a fixed-dose antihypertensive formulation and dissolution studies.

Cardiovascular diseases, especially hypertension, stand as prominent contributors to global mortality. Hypertension, often referred to as a silent killer syndrome, necessitates the use of multiple medications for effective control and management. A new environmentally friendly HPLC-DAD method is introduced in this study for the concurrent analysis of telmisartan (TEL), chlorthalidone (CHT) and amlodipine besylate (AML), in both pure forms and combined pharmaceutical dosage form. An isocratic elution mode was employed to achieve chromatographic separation, utilizing an Inertsil C18 column (250 × 4.6 mm, 5.0 µm) and a mobile phase mixture of acetonitrile and phosphate buffer (pH 3.0 ± 0.1) with ratio of 35:65, v/v. The separation was achieved within 10 min at a flow rate of 1.0 mL/min. The proposed method's validation was carried out following the guidelines outlined by the International Council for Harmonisation (ICH). The achieved linearity range was 1.0-140.0 µg/mL for TEL and 1.0-100.0 µg/mL for CHT and AML with quantification limits of 0.061, 0.177, and 0.313 µg/mL for TEL, CHT, and AML, respectively. The fixed combination tablet dosage form demonstrated acceptable release profile, as indicated by the in-vitro dissolution studies. The studied dissolution media were phosphate buffer pH 7.5, 0.01 N HCl, and water, utilizing a USP type II apparatus at 37 ± 0.5 °C with a stirring rate of 75 rpm. The proposed method was applied successfully for the quality assessment of Telma-ACT® Tablets with good precision and accuracy. Various tools were used for evaluating the level of greenness, including Green Analytical Procedure Index (GAPI), Analytical Greenness Metric for Sample Preparation (AGREEprep), Analytical Eco-Scale (AES), and Analytical Method Greenness Score (AMGS). These tools had confirmed the eco-friendliness of the proposed method. Additionally, the newly introduced White Analytical Chemistry (WAC), and the Blue Applicability Grade Index (BAGI) have been specifically developed to evaluate the sustainability and the applicability of the method.

Relatively reliable and rapid identification of colorant compounds in food matrices by HPLC-DAD-QTOF-MS combined with theoretical calculation.

A new convenient method for identifying colorant compounds (CCs) in food matrices was developed using high-performance liquid chromatography with a diode array detector and quadrupole-time-of-flight mass spectrometer (HPLC-DAD-Q/TOF-MS) combined with theoretical calculations. A model sample containing three typical CCs was completely separated via HPLC-DAD. The obtained 3D ultraviolet-visible (UV-vis) spectra revealed the maximum absorption wavelengths (MAWs) of all CCs (yellow, 430 nm; red, 520 nm; blue, 620 nm) in the range of 400-800 nm, and their colors were determined based on their MAWs. Temporary structures of the CCs were obtained using Q/TOF-MS analysis. Theoretical calculations were then performed to obtain the theoretical MAWs and colors of the CCs according to their calculated UV-vis spectra based on temporary structures. The structures of the CCs were confirmed without the need for authoritative standards by comparing the consistency between their experimental and theoretical MAWs and colors. This method is particularly suitable for identifying CCs or compounds with UV-Vis absorption, including new compounds, compounds for which standards are difficult to obtain, and known compounds without reporting relevant molecular information.

Phenolic compounds from pumpkin pulp: Extraction optimization and biological properties.

Ultrasound-assisted extraction of (poly)phenols from pumpkin pulp was optimized using response surface methodology. Time, solvent-to-sample ratio and percentage of water in ethanol were considered and a full factorial design was applied. The optimized conditions (10 min; 30 mL/g; 50% water in ethanol) were used to isolate (poly)phenols from five pumpkin varieties (Hokkaido, Lunga di Napoli, Mantovana, Moscata di Provenza, Violina rugosa), collected for two successive years. Phenolic acids were the most abundant phenolic class (gallic acid up to 413.50 µg/g), even if differences were observed among varieties and harvesting years. Generally, Violina rugosa harvested in 2021 showed the highest total phenol content (7.59 mg gallic acid equivalents/g) and antioxidant properties (16.93 mg Trolox equivalents/g). All pumpkin variety exhibited antimicrobial activity within a concentration range of 1.95 to 250 µg/mL. In conclusion, the pumpkin pulp can be considered a promising natural source of (poly)phenols for the development of health-promoting products.

Targeted Screening and Quantification of Characteristic Sesquiterpene Lactones in Ambrosia artemisiifolia L. at Different Growth Stages.

Sesquiterpene lactones are specialized plant metabolites with promising pharmacological activities. These metabolites are characteristic marker compounds for the aerial parts of Ambrosia artemisiifolia. Numerus sesquiterpene lactones have been isolated from ragweed; however, there is no information on their bioproduction and quantification throughout the life cycle of the plant. The sesquiterpene lactone content of ragweed samples collected in Szeged and Nyíri was analyzed using HPLC. Significant differences in the amount and bioproduction rhythm of sesquiterpene lactones were found between the two sets of samples. The samples collected near Szeged contained significantly lower amounts of the investigated compounds compared to the Nyíri samples. Sesquiterpene lactone production in the samples peaked at the end of July or in August; the trend of the change in sesquiterpene lactones might correlate with precipitation and temperature. Geographical location and geoclimatic factors might exert significant influence on the production of sesquiterpene lactones in ragweed.

Simultaneous determination of 11 water-soluble synthetic colorants in foods consumed in Chile by high-performance liquid chromatography with diode Array detection.

In Chile, limited information is available on colorants in commonly consumed foods among vulnerable age groups. We developed and validated a rapid HPLC-DAD method to simultaneously evaluate 11 synthetic colorants in candies, beverages, ice cream, and cereals. The method exhibited excellent analytical performance for all 11 colorants with LOD (0.44 - 1.55 mgL-1), LOQ v(1.32 - 4.70 mgL-1), precision (4.0 and 7.3% RSD), and recovery (80 - 105%) in fortified matrices (10-50-100 mgL-1). The highest detection frequencies were as follows: cereals > candies > beverages > ice cream. Sunset Yellow was the most prevalent colorant in all food matrices, followed by Allura Red and Azorubine. Positive samples contained between 1 and 5 synthetic colorants. With the exception of cereals, the colorant concentrations in the remaining matrices exceeded the Codex Alimentarius regulations and the values reported in other studies worldwide, indicating the Chilean population is at risk.

Chromatographic fingerprinting of ipratropium and fenoterol in their novel co-formulated inhaler treating major respiratory disorders; application to delivered dose uniformity testing along with greenness and whiteness assessment.

Ipratropium bromide (IPR) and fenoterol hydrobromide (FEN) have recently been combined in a promising inhaler to treat two prevalent inflammatory illnesses of the airways: bronchial asthma and chronic obstructive pulmonary disease (COPD). The necessity for a single, sensitive, and trustworthy analytical approach to cover the diverse and necessary tests of in-vitro and in-vivo studies is greatly grown with the rising production of new fixed combinations. Two novel, selective and environmentally friendly LC techniques were developed in order to guarantee precise measurement of IPR and FEN in their challenging formulation. The initial technique involved high-performance thin-layer chromatography (HPTLC) in conjunction with densitometric quantification. Chromatographic separation was attained on HPTLC plates utilizing ethyl acetate - ethanol - acetic acid (5.0:5.0:0.1, by volume) as a developing system. Densitometric quantification of the separated bands was carried out at 220.0 nm over concentration ranges of 0.50-15.0 µg/band for IPR and 0.50-12.0 µg/band for FEN. High-performance liquid chromatography (HPLC) paired with diode array detection (DAD) was the core of the second technique. The optimized separation was achieved on a Zorbax SB C18 (150 × 4.6 mm, 5 µm) column with a combination of 10.0 mM potassium dihydrogen orthophosphate, pH 5.0 ± 0.1, adjusted with o-phosphoric acid and methanol (70:30, v/v) as the mobile phase and pumped at flow rate of 1.0 mL/min. The peaks were monitored at 220.0 nm using diode array detection, achieving linearity range of 5.0-200.0 µg/mL for both drugs. The ICH criteria have been verified and both methods have been confirmed to be valid, and successfully applied for assay the cited drugs in the Atrovent® comp HFA metered dose inhaler as well as delivered dose uniformity testing of the final product. Finally, whiteness appraisal and several state-of-the-art green evaluation metrics were applied to evaluate the sustainability of the proposed methods. The suggested approaches produced promising results and are the first simple and sustainable methodologies for the simultaneous quantification of both drugs in different real samples, all of which strongly suggest their application in quality control laboratories.

Adulterated dietary supplements commercialized in Brazil: development of a screening method and a preliminary study of cytotoxicity.

The high consumption of dietary supplements was a fundamental driver for the creation of the regulatory framework by the Brazilian governmental authorities. However, the regulatory agencies lack official low-cost methodologies to evaluate the quality of food supplements. A preliminary screening method by HPLC-DAD was proposed and validated for screening and quantification of adulterants in dietary supplements. The limits of detection and quantification were <0.11 and 0.37 µg.g-1, respectively. The method was applied for the investigation of ten unauthorized substances (spironolactone, hydrochlorothiazide, furosemide, clenbuterol, testosterone, testosterone propionate, yohimbine, vardenafil, tadalafil, and sildenafil) with a time of analysis of <5 min. Sixteen percent of the 44 samples analyzed had at least one adulterant at or above therapeutic concentrations. Subsequently, in vitro evaluations were performed of the potential cytotoxicity to evaluate the cell viability, DNA damage, determination of nitric oxide levels, and quantification of reactive oxygen species. Despite the necessity of further studies, the results indicate a relationship between the presence of adulterants in food supplements and a potential cytotoxic effect.

Development and Validation of a High-Performance Liquid Chromatography Diode Array Detector Method to Measure Seven Neonicotinoids in Wheat.

Neonicotinoids (NEOs), used as insecticides against aphids, whiteflies, lepidopterans, and beetles, have numerous detrimental impacts on human health, including chronic illnesses, cancer, infertility, and birth anomalies. Monitoring the residues in food products is necessary to guarantee public health and ecological balance. The present work validated a new method to measure seven neonicotinoid insecticides (acetamiprid ACT, clothianidin CLT, dinotefuran DNT, imidacloprid IMD, nitenpyram NTP, thiacloprid TCP, and thiamethoxan THT) in wheat. The analytical procedure was based on simple and fast wheat sample cleanup using solid-phase extraction (SPE) to remove interferents and enrich the NEOs, alongside the NEOs' separation and quantification by reverse-phase chromatography coupled with a diode array detector (DAD). The validation process was validated using the accuracy profile strategy, a straightforward decision tool based on the measure of the total error (bias plus standard deviation) of the method. Our results proved that, in the future, at least 95% of the results obtained with the proposed method would fall within the ±15% acceptance limits. The test's cost-effectiveness, rapidity, and simplicity suggest its use for determining the levels of acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam in routine analyses of wheat.

Novel RP-HPLC-DAD approach for simultaneous determination of chlorphenoxamine hydrochloride and caffeine with their related substances.

Ensuring the quality control of active pharmaceutical ingredients is crucial for drug products being introduced into the market. Even for established drugs, it is necessary to maintain a cutting-edge impurity control system. To analyze caffeine and chlorphenoxamine hydrochloride in their binary mixture, as well as theophylline and chlorphenoxamine N-oxide as related substances, a reversed phase-high performance liquid chromatography combined with a diode array detector system was created. The chromatographic separation was conducted using a C18 X-select Waters® column. The mobile phase consisted of 20.0 mM potassium dihydrogen phosphate modified to pH 3 with o-phosphoric acid and methanol. A gradient elution program was adopted at a flow rate of 1.3 mL/min and detected at a wavelength of 222 nm. The present methodology demonstrates a concentration ranging from 2-60, 1-80, 0.5-20 to 0.4-20 µg/mL for chlorphenoxamine hydrochloride, caffeine, chlorphenoxamine N-Oxide and theophylline, respectively. Chlorphenoxamine N-Oxide, being an impurity of chlorphenoxamine was prepared by refluxing intact drug with 5% H2O2 for 24 h at 100 °C. One of the objectives of the analytical community is to promote the adoption of green analysis methods, which involve the development of environmentally friendly techniques. The levels of greenness and whiteness were evaluated using four specific tools: Eco-Scale System, GAPI, AGREE, and RGB tool. Furthermore, we have evaluated the greenness of the analytical method presented and compared its performance and greenness to that of the approach described in the literature. In this study, results from CPX and CAF analysis were compared to those obtained in a previous study. The result shows that there is no notable variation in precision and accuracy. The proposed method was validated in accordance with the requirements of ICH.

Derivative spectrophotometry-assisted determination of tryptophan metabolites emerges host and intestinal flora dysregulations during sepsis.

Sepsis is a life-threatening condition characterized by organ dysfunction resulting from a dysregulated host response to infection. Dysregulated tryptophan (TRP) metabolites serve as significant indicators for endogenous immune turnovers and abnormal metabolism in the intestinal microbiota during sepsis. Therefore, a high coverage determination of TRP and its metabolites in sepsis is beneficial for the diagnosis and prognosis of sepsis, as well as for understanding the underlying mechanism of sepsis development. However, similar structures in TRP metabolites make it challenging for separation and metabolite identification. Here, high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD) was developed to determine TRP metabolites in rat serum. The first-order derivative spectrophotometry of targeted metabolites in the serum was investigated and proved to be promising for chromatographic peak annotation across different columns and systems. The established method separating the targeted metabolites was optimized and validated to be sensitive and accurate. Application of the method revealed dysregulated TRP metabolites, associated with immune disorders and NAD + metabolism in both the host and gut flora in septic rats. Our findings indicate that the derivative spectrophotometry-assisted method enhances metabolite identifications for the chromatographic systems based on DAD detectors and holds promise for precision medicine in sepsis.

Discovery and determination of misuse and chemotypes of Pogostemon cablin by liquid chromatography-quadrupole time-of-flight mass spectrometry and liquid chromatography with diode-array detector.

Traditional Chinese medicine (TCM) has garnered significant scientific interest in healthcare but faces increased regulatory scrutiny due to concerns about uncontrolled usage. This study focuses on characterizing Pogostemon cablin (PC) to mitigate potential misuse and identify chemotype differences. Leveraging untargeted metabolomics, we identified 222 distinctive features effectively differentiating PC from Agastache rugosa (AR), reducing misidentification risks. Pogostone and tilianin emerged as potential markers, leading to a high-performance liquid chromatography-diode array detection (HPLC-DAD) method development for PC and AR discrimination. Evaluation of PC chromatograms revealed notable profile and pogostone level differences among samples, suggesting chemotype associations. Untargeted metabolic profiling identified 78 features with significant differences, highlighting 7,3',4'-tri-O-methyleriodictyol as a potential discriminatory marker between PC chemotypes. The developed HPLC-DAD method quantified pogostone and 7,3',4'-tri-O-methyleriodictyol, effectively discriminating PC chemotypes. This platform differentiates PC and AR and distinguishes chemical types within PC, like pogostone-type and patchoulol-type. Applied to local TCM stores, it ensures PC authenticity. This approach addresses TCM control concerns, enhancing understanding and application of herbal medicine by providing insights into PC chemical composition and discrimination.

Salvia miltiorrhiza bunge extracts: a promising source for anti-atopic dermatitis activity.

BACKGROUND: Atopic dermatitis (AD) is a chronic inflammatory condition characterized by the accumulation of reactive oxygen species and the expression of inflammatory factors. Regarding its anti-atopic activity, numerous traditional medicinal materials and secondary metabolic products play pivotal roles in modulating the associated mechanisms. METHODS: This study aimed to utilize Salvia miltiorrhiza Bunge (SMB) as an anti-AD source. In-vitro activity assessments and qualitative and quantitative analyses using UPLC-TQ-MS/MS and HPLC-DAD were conducted in two cultivars ('Dasan' and 'Kosan'). Statistical analysis indicated that the profiles of their secondary metabolites contribute significantly to their pharmacological properties. Consequently, bio-guided fractionation was undertaken to figure out the distinct roles of the secondary metabolites present in SMB. RESULTS: Comparative study of two cultivars indicated that 'Dasan', having higher salvianolic acid A and B, exhibited stronger antioxidant and anti-inflammatory activities. Meanwhile, 'Kosan', containing higher tanshinones, showed higher alleviating activities on anti-AD related genes in mRNA levels. Additionally, performed bio-guided fractionation re-confirmed that the hydrophilic compounds of SMB can prevent AD by inhibiting accumulation of ROS and suppressing inflammatory factors and the lipophilic components can directly inhibit AD. CONCLUSIONS: SMB was revealed as a good source for anti-AD activity. Several bioactive compounds were identified from the UPLC-TQ-MS/MS and different compounds content was linked to biological activities. Characterization of these compounds may be helpful to understand differential role of secondary metabolites from SMB on alleviation of AD.