Search

Yeonkyopaedok-san is a traditional Korean medicine used in the early treatment of boils. In the present study, its 12 marker components for quality control were determined using high-performance liquid chromatography (HPLC) with photodiode array detection and ultra-performance liquid chromatography–mass spectrometry with tandem mass spectrometry (UPLC–MS/MS). The investigated 12 marker components of Yeonkyopaedok-san were as follows: 3-caffeoylquinic acid, cimifugin 7-glucoside, liquiritin apioside, ferulic acid, narirutin, 5-O-methylvisammioside, naringin, neohesperidin, oxypeucedanin hydrate, arctigenin, glycyrrhizic acid, and 6-gingerol. The analytical column used for the separation of the 12 marker analytes in Yeonkyopaedok-san was a Waters SunFire C18 column (4.6 mm × 250 mm, 5 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and 0.1% (v/v) formic acid in acetonitrile. In the UPLC–MS/MS analysis, all components were separated using a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and acetonitrile. The coefficient of determination of the calibration curves in both analysis systems showed good linearity (>0.99). The amounts of the 12 marker components in Yeonkyopaedok-san determined using HPLC–photodiode array detection and UPLC–MS/MS analyses were found to be 0.14–9.00 mg/g and 2.35–853.11 μg/g, respectively. [ABSTRACT FROM AUTHOR]

Compound amino acid injection-18 AA (CAAI-18 AA) is widely applied in medical care as a part of total parenteral nutrition systems. Thus, suitable quality control of CAAI-18 AA is of crucial importance for safety of the patients. Tryptophan (TRP) is one of the main components in CAAI-18 AA and may be degraded to 5-hydroxy-tryptophan (5-HTP), 5-hydroxytryptamine (5-HT), kynurenine (KYN) and indole (IN) under certain conditions, such as oxidation environments, ultraviolet light radiation and nonsterile conditions. The existence of these harmful impurities seriously affects the quality of CAAI-18 AA. Here, a simple HPLC approach with a PDA detector was developed and validated for simultaneous determination of the concentrations of 5-HTP, 5-HT, KYN and IN impurities in CAAI-18 AA. Separation of these four impurities in CAAI-18 AA was achieved under a gradient condition using acetonitrile and 10 mM phosphate buffer (containing 10 mM sodium 1-octanesulfonate, pH adjusted to 1.8 with phosphoric acid). To detect the four analytes with high sensitivity, multi-wavelength detection at 257, 270 and 276 nm was carried out during the separation. The method was validated in accordance with ICH guidelines and the results were compared to that obtained by UHPLC–MS/MS, showing that the two approaches did not provide significantly different results. Our results reveal that the simple and less expensive HPLC method holds great potential for quantitation of the four impurities in CAAI-18 AA. [ABSTRACT FROM AUTHOR]

Parabens are widely used as preservatives in thousands of consumer's products including, cosmetics, pharmaceutical products, and foodstuffs. Concern in regards to the safety of parabens has been raised where parabens have been classified as "Endocrine disrupting compounds" with potential link to many tumor types. Despite their wide spread, the occurrence of parabens in foodstuffs available in the Saudi market has not been studied until now. In this work, an HPLC-PDA method was developed and validated for the screening of parabens' residues in different categories of Ready-to-eat foodstuffs collected from the Saudi market. These categories include: cereals, meat, fish, dairy product, bean products, fruits, vegetables, cookies and snacks, beverages, condiments, and others. Chromatographic analysis of the selected parabens (Methyl paraben MeP, ethyl paraben EtP, propyl paraben PrP, butyl paraben BuP, and isobutyl paraben isoBuP) was performed on Symmetry® C-18 Colum (4.6 × 75 mm, 3.5 μm) with methanol/water (57:43, v/v) as the mobile phase and using simply methanol for sample preparation. The proposed method was fully validated with regards to linearity, limits of detection (LOD) and of quantitation (LOQ), accuracy and precision, extraction recovery, and specificity. Matrix-based calibration curves were linear in the range 0.025–500 μg/g (MeP, EtP), 0.05–500 μg/g (PrP), and 0.125–1250 μg/g (IsoBuP, BuP) with LOQ 0.025 μg/g for MeP, EtP, 0.05 μg/g for PrP, 0.125 μg/g for both BuP and isoBuP. The method was successfully applied for quantitative screening of the five parabens in different Ready-to-eat foodstuffs (n = 215) collected from the Saudi market. The total parabens content was determined and was related to the food category and to the packaging material. The highest paraben content was found in cereals and condiments. The type of the packaging material did not have a significant effect on the paraben content among all food categories. Moreover, the estimated daily intake of parabens among the Saudi adults was calculated and it was found to have an average of 2000 μg/kgbw/day. [ABSTRACT FROM AUTHOR]

Anti-inflammatory agents may be alternatives for the treatment of Alzheimer's disease. Then, we propose the nanotechnology as a strategy to curcumin and meloxicam co-nanoencapsulation for neurodegenerative diseases treatment. In this study, we developed and validated an analytical method by HPLC-DAD for simultaneous quantification of curcumin and meloxicam in the same formulation. We applied this method to characterize curcumin, meloxican and curcumin plus meloxican loaded lipid-core nanocapsules (LNC): drug content, encapsulation efficiency, photostability and drug's distribution. Additionally, toxicity levels of the nanoparticles were evaluated in vivo (mice). Therefore a C 18 -RP column was used with a guard column packed with the same material as the stationary phase. Acetonitrile: methanol: water: triethylamine (52:5:43:0.3 v/v/v/v), was used as the mobile phase in the 1 mL min−1 flow. Detection was 424 nm (curcumin) and 365 nm (meloxicam). The method was established in accordance with the current national and international guidelines, showing good linearity (r2 > 0.999). The formulations showed exclusively nanosized particles, negative zeta potential and slightly acidic pH, with content and encapsulation rate close to 100%. The distributions of meloxicam and curcumin in the LNC (alone or co-encapsulated) were type III and type VI, respectively. LNC were able to protect both drugs against UVA degradation. In vivo experiments showed no toxicity in relation to the parameters determined of all LNC evaluated in mice. In this work, we showed the possibility to carry meloxicam and curcumin in LNC with good technological characteristics and without toxicity in vivo with prospects for the treatment of Alzheimer's disease in sequential pharmacological studies. [ABSTRACT FROM AUTHOR]

Lingonberry leaves have been proposed as a potential raw material for nutraceutical products and functional food due to the richness of phenolic and triterpenic compounds. However, contents of these bioactive compounds tend to vary greatly with physiological, climatic, and edaphic conditions, resulting in lingonberry leaves’ nutritional-pharmaceutical quality changes. In this context, we examined the effects of seasonal and geographical factors on phenolic and triterpenoid contents in lingonberry leaves. Quantitative and qualitative differences between samples were determined using validated HPLC-PDA methods. A total of 43 bioactive compounds were found at a detectable level throughout the year in young and old lingonberry leaves, with the highest contents of most compounds observed in samples collected in autumn–first half of spring. This suggests the potential to exploit the continuous biosynthesis for a longer harvesting season. Considerable variations in phytochemical profiles of lingonberry leaves, obtained from 28 locations in Lithuania, were found. Correlation analyses revealed significant negative correlations between contents of particular constituents and sunshine duration, temperature, and precipitation, and positive correlation with air humidity, longitudes, and altitudes of collecting locations and macronutrients in soil. These results suggest that harsh weather is favorable for most identified compounds and it may be possible to achieve appropriate accumulation of secondary metabolites by adjusting edaphic conditions. Taken together, the accumulation of phenolics and triterpenoids in lingonberry leaves highly depends on phenological and geographical factors and the influence of both variables differ for the particular compounds due to different metabolic processes in response to stresses.

Propolis is a resinous natural product collected by honeybees (Apis mellifera and others) from tree exudates that has been widely used in folk medicine. The present study was carried out to investigate the fatty acid composition, chemical constituents, antioxidant, and xanthine oxidase (XO) inhibitory activity of Jordanian propolis, collected from Al-Ghour, Jordan. The hexane extract of Jordanian propolis contained different fatty acids, which are reported for the first time by using GC-FID. The HPLC was carried out to identify important chemical constituents such as fatty acids, polyphenols and α-tocopherol. The antioxidant and xanthine oxidase inhibitory activities were also monitored. The major fatty acid identified were palmitic acid (44.6%), oleic acid (18:1∆9cis, 24.6%), arachidic acid (7.4%), stearic acid (5.4%), linoleic acid (18:2∆9–12cis, 3.1%), caprylic acid (2.9%), lignoceric acid (2.6%), cis-11,14-eicosaldienoic acid (20:2∆11–14cis, 2.4%), palmitoleic acid (1.5%), cis-11-eicosenoic acid (1.2%), α–linolenic acid (18:3∆9–12–15cis, 1.1%), cis-13,16-docosadienoic acid (22:2∆13–16cis, 1.0%), along with other fatty acids. The major chemical constituents identified using gradient HPLC-PDA analysis were pinocembrin (2.82%), chrysin (1.83%), luteolin-7-O-glucoside (1.23%), caffeic acid (1.12%), caffeic acid phenethyl ester (CAPE, 0.79%), apigenin (0.54%), galangin (0.46%), and luteolin (0.30%); while the minor constituents were hesperidin, quercetin, rutin, and vanillic acid. The percentage of α-tocopherol was 2.01 µg/g of the lipid fraction of propolis. Antioxidant properties of the extracts were determined via DPPH radical scavenging. The DPPH radical scavenging activities (IC50) of different extracts ranged from 6.13 to 60.5 µg/mL compared to ascorbic acid (1.21 µg/mL). The xanthine oxidase inhibition (IC50) ranged from 75.11 to 250.74 µg/mL compared to allopurinol (0.38 µg/mL). The results indicate that the various flavonoids, phenolic compounds, α-tocopherol, and other constituents which are present in propolis are responsible for the antioxidant and xanthine oxidation inhibition activity. To evaluate the safety studies of propolis, the pesticide residues were also monitored by LC-MS-MS 4500 Q-Trap. Trace amounts of pesticide residue (ng/mL) were detected in the samples, which are far below the permissible limit as per international guidelines.

In this study, five silk fabrics were separately dyed with madder (Rubia tinctorium L.) and gallnut (Quercus infectoria Olivier) in different percentages and then tested for antifungal activity against Candida albicans DSMZ 1386. The one having highest antifungal activity was washed 5 times under same conditions and samples were taken after every wash. They retained nearly 99.98 % activity up to five launderings against Candida albicans. In addition, coloring compounds and their peak heights in dyed silk fabrics were detected by high performance liquid chromatography with diode array detection (HPLC-PDA). Color values of the dyed silk fabrics were measured by CIEL*a*b* spectrophotometer.

Abstract. In this study the rate of accumulation of both main pigments in Salmonidae - astaxanthin (AX) and canthaxanthin (CX) in different muscle tissues of Rainbow trout (Oncorhynchus mykiss W.) and their distribution in flesh and heart was researched. Experimental fish were reared 100 days in two tanks as two -1 -1 parallel experimental groups and fed with market feed, containing 40 mg.kg AX and 25 mg.kg CX. The diet was according to the manufacturer's recommendations, which are consistent with fish size and water temperature. The accumulated pigment quantities in the muscle tissues, were measured every twenty days by high performance liquid chromatography with photodiode array detection after selective xanthophyll extraction. The highest rates of AX th th -1 and CX deposition were recorded on the 60 and 80 day. The average contents of AX and CX were at the end of the trial 1.943 ± 0.167 mg.kg and 0.807 ± -1 -1 -1 0.021 mg.kg in skeletal muscle and 0.683 ±0.055mg.kg and 0.280 ±0.017 mg.kg in cardio muscle, respectively.

Insamyangpye–tang (ISYPT) is a traditional medicinal formula comprised of 13 herbs and has been used in East Asia to treat lung-related diseases. However, to our knowledge, no method of analysis for its quality control has been reported. In this study, a method of analysis for quality control of ISYPT was developed using high-performance liquid chromatography. Chromatographic separation, analysis, and assay verification were performed with a distilled water–acetonitrile mobile phase system, both containing 0.1% (v/v) trifluoroacetic acid, and a Gemini C18 analytical column (4.6 mm × 250 mm, 5 μm) using authentic standards for eight marker compounds. These marker constituents were detected simultaneously at 0.09–5.95 mg/g. The analysis method developed can be used for basic quality control of ISYPT.

Custard apple is an edible fruit grown in tropical and subtropical regions. Due to its abundant nutrient content and perceived health benefits, it is a popular food for consumption and is utilized as a medicinal aid. Although some published research had provided the phenolic compound of custard apple, the comprehensive phenolic profiling of Australian grown custard apple is limited. Hence, this research aimed to evaluate the phenolic content and antioxidant potential by various phenolic content and antioxidant assays, followed by characterization and quantification of the phenolic profile using LC-ESI-QTOF-MS/MS and HPLC-PDA. African Pride peel had the highest value in TPC (61.69 ± 1.48 mg GAE/g), TFC (0.42 ± 0.01 mg QE/g) and TTC (43.25 ± 6.70 mg CE/g), followed by Pink’s Mammoth peel (19.37 ± 1.48 mg GAE/g for TPC, 0.27 ± 0.03 mg QE/g for TFC and 10.25 ± 1.13 mg CE/g for TTC). African Pride peel also exhibited the highest antioxidant potential for TAC (43.41 ± 1.66 mg AAE/g), FRAP (3.60 ± 0.14 mg AAE/g) and ABTS (127.67 ± 4.60 mg AAE/g), whereas Pink’s Mammoth peel had the highest DPPH (16.09 ± 0.34 mg AAE/g), RPA (5.32 ± 0.14 mg AAE/g), •OH-RSA (1.23 ± 0.25 mg AAE/g) and FICA (3.17 ± 0.18 mg EDTA/g). LC-ESI-QTOF-MS/MS experiment successfully characterized 85 phenolic compounds in total, encompassing phenolic acids (20), flavonoids (42), stilbenes (4), lignans (6) and other polyphenols (13) in all three parts (pulp, peel and seeds) of custard apple. The phenolic compounds in different portions of custard apples were quantified by HPLC-PDA, and it was shown that African Pride peel had higher concentrations of the most abundant phenolics. This is the first study to provide the comprehensive phenolic profile of Australian grown custard apples, and the results highlight that each part of custard apple can be a rich source of phenolics for the utilization of custard apple fruit and waste in the food, animal feeding and nutraceutical industries.

This study describes the possibilities of valorising a waste stream that originates from apple wood by mapping the reducing capacity and phenolic profile from extracts derived from apple tree (Malus domestica). This study evaluated the efficiency of warm solvent extraction (WSE) and ultrasound-assisted extraction (UAE) techniques for extracting antioxidant phenolic compounds from the bark and core wood of an apple tree cultivated in the north-eastern part of Belgium. Furthermore, the influence of the pre-treatment technique, namely, fresh, oven-dried, and freeze-dried samples, respectively, on the yield of polyphenols was studied. Fresh bark extract obtained by UAE—the most efficient extraction technique—employing acetone 60% v/v contains the highest levels of phenolic compounds as well as the highest antioxidant activity. High-performance liquid chromatographic analysis shows that phloridzin is the major compound of the identified polyphenol markers present in bark and core wood extracts. Based on the obtained results, it may be possible to produce a polyphenolic extract from apple wood at an industrial scale without extensive costs or altering the antioxidant properties. This study reveals the potential of apple tree wood residues valorisation through the recovery of phenolic compounds for food, pharmaceutical, and cosmetic applications. [ABSTRACT FROM AUTHOR]

Cynoglossum creticum Mill (Boraginaceae) is used traditionally as a remedy to manage several human ailments. In this context, the present study aimed to perform multiple pharmacological investigations on the hydroalcoholic extracts prepared from Cynoglossum roots and aerial parts (leaves and flowers). We evaluated the antioxidant and enzyme inhibitory (against cholinesterases, α-glucosidase, α-amylase, lipase and tyrosinase) activity of the extracts. The protective effect(s) of the extracts on cardiomyocyte C2C12 and intestinal HCT116 cell lines challenged with hydrogen peroxide (H2O2) was studied. We found that the aerial parts harbored the highest amount of phenolic compounds. Generally, aerial parts showed significant antioxidant and enzyme inhibitory effects. Leaves exhibited the best lipase inhibitory activity (173.15 mgOE/g extract), followed by flowers and roots. The root and aerial extracts were equally able to blunt intracellular H2O2 induced reactive oxygen species production from both C2C12 and HCT116 cell lines. Both cells lines could be treated with scalar concentrations of root and flower extracts in the range 50–300 μg/mL without interferences on cell viability. In conclusion, the present study showed protective effects exerted by Cynoglossum extracts, which could serve as a foundation for the development of pharmaceuticals and nutraceuticals derived from Cynoglossum. [ABSTRACT FROM AUTHOR]

Introduction: Clerodendrum petasites (Lour.) S. Moore (locally known as Mai-Thao-Yaai-Mom), belonging to the Verbenaceae family, is widely formulated into multi-herb remedy, Ben-Cha-Lo-Ka-Wi-Chian remedy, possessing antipyretic activity. C. petasites exhibits many biological activities, such as antioxidant, anti-inflammatory, antipyretic, etc. The flavonoid hispidulin is one of the main active compounds present in C. petasites, containing anti-atheromatous, antitumor and antispasmodic effects. Objective: The present study aimed to determine the hispidulin content in the dried roots of C. petasites using HPLC technique. Methods: C. petasites dried roots, collected from twelve different areas, were extracted with ethanol using Soxhlet apparatus, and then subjected to HPLC-PDA to quantify hispidulin content. The quantitative method using HPLC-PDA technique was validated. Results: The optimized HPLC coupling with PDA detector (HPLC-PDA) was validated for the quantitative analysis of hispidulin content in C. petasites roots in terms of linearity (y = 210,200,536.6667x - 448,756.2667; R2 = 0.9997), accuracy (88.82-107.69% recovery), precision (0.66% RSD for repeatability precision; 1.17% RSD for intermediate precision), limit of detection (2.30 µg/mL), limit of quantitation (7.00 µg/mL), specificity (peak purity index = 1.0000) and robustness (% RSD < 1). The amount of hispidulin content in the extracts of C. petasites roots conducted from the validated method was found to be 0.0182 ± 0.0109 g/100 g crude drug. Conclusion: The HPLC-PDA analysis was able to effectively determine hispidulin in C. petasites roots. The hispidulin contents in C. petasites dried roots from various areas in Thailand were revealed which could be used for the specification of this crude drug with reference to its chemical marker. [ABSTRACT FROM AUTHOR]

A simple and efficient ultrasonic-assisted extraction (UAE) technique was developed in order to find optimal conditions for the extraction of total phenolic compounds, flavonoids and anthocyanins in wild raspberry (Rubus idaeus L.) fruits. Several extraction variables, including methanol composition (v/v, %), solid-solvent ratio (g/mL), time (min) and extraction temperature (°C) were optimized using response surface methodology (RSM). Under optimal conditions for extraction, the total phenolics were found in the concentration of 383 mg GAE/100 g of fresh fruit weight, while HPLC-PDA analysis of the optimized extract showed the presence of cyanidin-3-glucoside, cyanidin-3-sophoroside, catechin, gallic and ellagic acid. The experimental values of DPPH and ABTS radical scavenging activities were 29.0 and 39.5 μmol Trolox/g of fresh fruit weight, respectively. In vitro simulated gastrointestinal digestion showed great raspberry phenolics stability. Our study assessed the bioaccessible phenolics in wild raspberry fruits and showed optimal conditions for the effective extraction of bioactive compounds for their analysis. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • Sesamin and sesamolin were rapidly quantified in sesame seeds by HPTLC. • A green approach, compatible with EU Pharmacopoeia, was implemented. • Results were compared with a validated HPLC-PDA protocol. • HPTLC densitometry proves to be an effective alternative to HPLC-PDA. Abstract Sesamin and sesamolin constitute the main bioactive secondary metabolites of sesame seeds (Sesamum indicum L., Pedaliaceae). In the present work, a rapid HPTLC-based methodology was developed in compliance with the requirements of the European Pharmacopoeia for the quantification of these two lignans in sesame seeds. A comparative study was simultaneously performed with HPLC-PDA for assessing the sesamin and sesamolin content of diverse samples. Both methods were validated and the results were subsequently subjected to statistical analysis in order to compare their performance as well as to investigate possible correlations. The methods were shown to be adequately correlated in terms of performance, as revealed by Pearson's rank correlation coefficients (>0.99 for sesamin and >0.98 for sesamolin) and Bland-Altman analysis (relative method bias 0.06–0.21, SD of bias 0.05–0.07). HPTLC densitometry could thereby serve as a valid and reliable tool for the rapid determination of the major lignans in sesame seed samples. [ABSTRACT FROM AUTHOR]

Safflower is well-known by textile conservators and restorers as the red dye source that produces a nice, though very delicate pink colour that is extremely light-sensitive. The fading due to light sensitivity can be seen in many historical silk fabrics from the most renowned museums and it is a major challenge for textile conservators. However, the fading is not only a result of light exposure, as fabrics stored for many years in dark museum storage also exhibit gradual decolouration. The aim of this study is to increase knowledge on the environmental parameters involved in the degradation processes of carthamin, the main red dye constituent of safflower (Carthamus tinctorius L.). The newly gained information will contribute to a more realistic perspective on the problems of fading of safflower-dyed textiles, possibly helping their conservation. To evaluate the stability of safflower red, specific ageing tests were carried out on new silk samples, dyed with safflower through modern recipes deriving from traditional ones. For the artificial ageing, the effects of simulated sunlight, temperature, humidity and ozone were separately investigated through HPLC-PDA analysis and colorimetric examinations. The results confirmed that safflower red degrades most rapidly under light exposure. They also revealed an important instability of the carthamin dye constituent in a dark environment, especially when subjected to high humidity conditions. Moreover, the HPLC-PDA study was able to provide new insight into the different markers (e.g. Ct components) that are commonly revealed in historic objects dyed with safflower red, but that still have unclarified origins. [ABSTRACT FROM AUTHOR]

Aronia melanocarpa is a rich source of phenolic compounds like anthocyanins, chlorogenic acids, quercetin derivatives, and proanthocyanidins possessing strong antioxidative potential. The consumption of A. melanocarpa is actually increasing because of the known bioactivity of its phenolic constituents. A. melanocarpa extracts are used as natural colorants and nutraceuticals. Several attempts of adulteration of aronia products have already been reported. In this study, we investigated changes in phenolic composition from berry to juice by HPLC‐PDA, and HPLC‐ESI‐MSn analyses as well as fingerprint profiles for authentication of commercially available aronia products in order to detect possible adulteration. Additionally, the radical scavenging activity of aronia products was determined by using the TEAC (Trolox® equivalent antioxidant capacity) assay. Aronia pomace, a valuable by‐product of juice production, showed the highest phenolic content and possessed the highest radical scavenging activity. [ABSTRACT FROM AUTHOR]

Abstract Pyriproxyfen (PPF) is a larvicide, used to combat the proliferation of Aedes aegypti larvae. The objective of this study was to analyze the compounds of pyriproxyfen and pyridalyl (PYL) in a commercial larvicide to analyze the cytotoxic and oxidative effects of PPF and PYL. The toxic potential of PPF and PYL were assessed based on lethal concentration (LC 50) in Artemia salina , cytotoxicity based on the mitotic index and the chromosomal alterations in Allium cepa and the oxidative damage in Saccharomyces cerevisiae. The PPF and PYL compounds were identified by HPLC-PDA based on their retention times and spectral data. The wavelengths λ max (258 nm) and (271 nm) of the UV spectrum of PYL and PPF and the retention times (R T) (3.38 min) and (4.03 min), respectively. The toxicological potentials of PPF and PYL were significant at concentrations (1, 10, 100 and 1000 ppm), with an LC 50 of 48 h (0.5 ppm). PPF and PYL pointed out a cytotoxic effect in A. cepa at all concentrations (0.0001, 0.001, 0.01, 0.1, 1.0, 100 and 1000 ppm), genotoxic effect at concentrations only (0.0001; 0.1; 1; 100 and 1000 ppm), and mutagenic for concentrations (0.1, 100 and 1000 ppm). In relation S. cerevisiae , PPF e PYL prompted oxidative damage at concentrations (100 and 1000 ppm) in all strains (SODWT, Sod1 , Sod2 , Sod1Sod2 , Cat1 and Sod1Cat1). Therefore, the PPF and PYL identificated in commercial larvicide by HPLC-PDA produced cytotoxic and oxidative effects that could cause health and ecosystem risks. Graphical abstract Image 1047749 Highlights • In chromatography the pyriproxyfen is was the major product of the mixture. • PFF and PYL presented toxic, cytotoxic, genotoxic and oxidative effects in high concentration. • The indiscriminate use of pesticides may pose a risk to the environment. [ABSTRACT FROM AUTHOR]

The carotenoid profiles of biomass from five eukaryotic microalgae, Porphyridium cruentum, Isochrysis galbana, Phaeodactylum tricornutum, Tetraselmis suecica and Nannochloropsis gaditana, produced at an industrial plant in outdoor photobioreactors, were investigated. Pigments were solvent-extracted after an ultrasonic pre-treatment and separated by HPLC-photodiode-array using a reversed-phase C18 column. Microalgae showed species-specific carotenoid profiles. Carotenoids were mostly in their free form, with a prevalence of xanthophylls over carotenes. Beta-carotene was the only carotenoid common to all species. The Rhodophyta P. cruentum exhibited the lowest total carotenoid content (167.2 mg 100 g−1 dw) and the simplest profile, with (all- E)-zeaxanthin (94.2 mg 100 g−1 dw, 56% of total carotenoids) and (all- E)- β – carotene (53.4 mg 100 g−1 dw, 32% of total carotenoids) as the major carotenoids. The Haptophyta Isochrysis galbana and the Bacillariophyta Phaeodactylum tricornutum were the species with the highest total carotenoid content (1760 mg and 1022 mg 100 g−1 dw, respectively). These species were characterized by similar carotenoid profiles, with (all- E)-fucoxanthin as the chief compound (1346 mg and 776.8 mg 100 g−1 dw for I. galbana and P. tricornutum , respectively), accounting for about 76% of total carotenoids. The Chlorophyta Tetraselmis suecica was the species showing the greatest variety of carotenoids, with both α - carotene and β - carotene and their derivatives present. (All- E)-lutein (85.4 mg 100 g−1 dw) and (all- E)-violaxanthin (81.8 mg 100 g−1 dw) were the major pigments in this species. In the Ochrophyta Nannochloropsis gaditana, (all- E)-violaxanthin was the prevalent carotenoid (336.7 mg 100 g−1 dw), followed by (all- E)-β-carotene (100.1 mg 100 g−1 algal dw). The carotenoid content of the microalgal biomass studied compared favourably to that of major vegetable sources. Due to their characteristics, these microalgae, most of them currently finding their main application in aquaculture, may be also regarded as valuable sources of carotenoids to be used in the formulation of functional food and nutraceuticals. Unlabelled Image • Microalgae showed species-specific carotenoid profiles. • Carotenoids were mostly in their free form, with a prevalence of xanthophylls over carotenes. • β-carotene was the only carotenoid common to all species. • Carotenoid levels compared favourably to those of high food sources. [ABSTRACT FROM AUTHOR]

Highlights • Simultaneous HPLC analysis of sodium iron/sodium copper chlorophyllins (SIC/SCC). • Inertsil ODS-2 column and methanol/water/acetic acid mobile phase used in HPLC. • Detection performed at wavelength of 395 nm. • Main components were Fe-isochlorine e4 (for SIC) and Cu-isochlorine e4 (for SCC). Abstract A simultaneous method for analyzing sodium iron chlorophyllin (SIC) and sodium copper chlorophyllin (SCC) using high-performance liquid chromatography was developed. This method employed an Inertsil ODS-2 column and diode array detection at 395 nm, using methanol–water (97:3 and 80:20, v/v) containing 1% acetic acid as the mobile phase. Liquid chromatography–tandem mass spectrometry was used to identify the main components of SIC and SCC as Fe-isochlorine e4 and Cu-isochlorine e4, respectively. The limits of detection and quantitation of SIC were 1.2 and 4.1 mg/kg, respectively, while those of SCC were 1.4 and 4.8 mg/kg, respectively. For intraday and interday tests, the SIC recoveries from candy ranged from 81% to 101%, while SCC recoveries ranged from 100% to 109%. The developed method can be applied to the rapid determination of SIC and SCC in candy. [ABSTRACT FROM AUTHOR]

Despite the importance of aquaculture increases for feeding the growing world population, professional farm management and proper use of aquaculture products or drugs are needed. It is important to know the quality of commercial antimicrobial products on the market while there is wide use of antimicrobials to treat fish diseases. The most commonly used antimicrobial products were identified from a previous survey, included amoxicillin, enrofloxacin, florfenicol, sulphadiazine, sulphamonomethoxine and sulphadimidine. Eight local chemical supply shops were randomly sampled in representative aquaculture areas in Maoming and Zhanjiang districts of south China in 2013. In this study, only eight products contained active substances within ±10% of the concentration declared on the product label among the 30 different most used commercial products; while six products did not contain any of the declared antimicrobials. Three products without labels were sold as 'pure antimicrobial' and had high concentrations of active antimicrobials. Furthermore, most products only provided ambiguous information on the packages on both antimicrobial usage and dosage; and only one product stated how to prepare medicated feed which is important for efficient usage. The results of this study showed that the aquaculture antimicrobial products sold on the market were of low quality and thus compromised effective fish disease treatment. Moreover, insufficient information on products' labels would provide limited instruction on correct antimicrobial usage. Inspection and supervision by both private companies and the government's sector require strengthening. [ABSTRACT FROM AUTHOR]

Abstract: Dissolution testing is a very significant tool that adds in vivo relevance to in vitro analytical data, thus providing a realistic in vitro/in vivo correlation. Dissolution profiling serves as a predictor of biological performance since the rate limiting step in the absorption of any drug is the rate of release from its pharmaceutical formulation. Being a routine procedure in quality control laboratories for initial approval process and scaling-up, the development of more and more eco-friendly methods for dissolution monitoring is considered as a worldwide trendy goal. In the present contribution, a comparison was highlighted between the two analytical techniques of utmost importance in acquisition of dissolution profiles: UV-spectrophotometry and HPLC-PDA focusing on the greenness of each one for further consolidation of the biowaiver concept. Both techniques were applied on the recently FDA-approved combination naproxen sodium (NAPR) and diphenhydramine hydrochloride (DIPH) formulated as Aleve pm® tablets. For the first time, this binary mixture was analyzed by three UV-spectrophotometric methods. NAPR was directly determined by zero-order spectrophotometry at 330 nm, where the spectrum of DIPH shows zero contribution. Whereas DIPH was determined by three simple methods exploiting the ratio spectra calculated using the spectrum of 20 µg/ml NAPR as a divisor. The first proposed method was ratio difference (RD), the second was ratio subtraction, and the last one was derivative ratio method. Being the simplest method, RD was the spectrophotometric method of choice that was applied in monitoring the dissolution of DIPH from Aleve pm® tablets. Although RD method has been widely described in many publications dealing with pharmaceutical analysis, it is the first article that opens a new horizon for RD method in the way of being a real-life application rather than only a method for determination. The second technique was a previously published HPLC-PDA, in which dissolution was then monitored by calculating the peak area of each component drug over time. Methods' validation was performed agreeing with the ICH guidelines. The advantages and challenges of each technique are discussed in a side-by-side comparison giving a key to recognize which one can positively influence environmental well-being.Graphical abstract: [ABSTRACT FROM AUTHOR]

Abstract An Italian certified Neem seed oil was characterized through the color analysis, the HPLC phenolic fingerprint and the preliminary evaluation of the cytotoxicity profile against the human macrophage (THP-1) cell line. Moreover, a wide screening of its enzyme inhibitory profile, antimicrobial activity towards Helicobacter pylori , several Candida spp. and Malassezia furfur strains and antiprotozoal activity against Plasmodium falciparum , Leishmania infantum and Leishmania tropica were performed. Neem seed oil demonstrated low toxicity and a great inhibitory efficacy against tyrosinase and lipase enzymes. Antimalarial and anti-leishmanial activities were also demonstrated, but weak or no activity was evidenced against Helicobacter pylori , Candida and Malassezia strains. Overall, these findings encourage the potential use of this natural product in some disease treatments and justify its use in traditional medicine. Highlights • Neem oil was analyzed by HPLC-PDA and color parameters. • Neem oil was inactive against Candida spp. and Malassezia furfur. • Neem oil displayed a discrete antimalaria and anti- Leishmania activity. • Lipase and tyrosinase were strongly inhibited by Neem oil. • Cytotoxicity against THP-1 cell line was assessed by MTT assay. [ABSTRACT FROM AUTHOR]

Granny Smith apples can be consumed as fresh or they are widely used in the frozen food industry. Determining the changes in polyphenol content during the production steps of foods is important for the nutritional value of the final product. The aim of this study was to determine the changes in the polyphenol content of Granny Smith apples taken from various steps of the individual quick freezing (IQF) treatment. Total phenolic content, total flavonoid content, and total antioxidant capacity were determined using spectrophotometric methods whereas the quantification of polyphenols were carried out by a chromatographic method using high performance liquid chromatography- photodiode array detector (HPLC-PDA). As a result of HPLC-PDA analysis, a total of 10 polyphenolic compounds belonging to 4 groups including flavanols, dihydrochalcones, phenolic acids and flavonols were identified in the raw material. Waste product was richer in dihydrochalcones and flavonols compared to raw material (140-378%) (p<0.05). Acidification resulted in significant increases in total phenolic content, total flavonoid content, total antioxidant capacity, flavanols and phenolic acids (%9-121) (p<0.05). Although there were decreases after cutting and freezing steps compared to acidification, there was no statistically significant difference between the raw material and end product in terms of the total phenolic content, total flavonoid content, flavanols, dihydrochalcones and phenolic acids (p>0.05). These results indicated that IQF Granny Smith apples are good sources of polyphenols, just as fresh apples. [ABSTRACT FROM AUTHOR]

Highlights • Evaluated the composition of polyphenols in fruits from 90 cultivars of F. ananassa. • Eighty of cultivars were analyzed for the first time. • Tannins and ellagitannins had the greatest influence on antioxidant activity. • Cultivars with a high content of tannins and high antioxidant capacity were selected. Abstract Strawberry fruit is a valuable resource, rich in vitamins and polyphenolic compounds. These compounds have a broad spectrum of biological activity. The aim of this study was to evaluate the qualitative and quantitative composition of polyphenols in strawberry fruit from 90 cultivars of Fragaria × ananassa Duch. from two growing seasons. Eighty of them were analyzed for the first time (to the best of our knowledge). The identification of polyphenolics and other compounds was performed using UPLC-qTOF-MS/MS. Nine compounds were recorded for the first time in mature strawberry fruit. Antioxidant properties were also determined using DPPH and ABTS methods. Statistical analysis of the results was performed using principal component analysis. Tannins, especially ellagitannins with agrimoniin, as well as the total polyphenols, had the greatest influence on antioxidant activity in the ABTS test. Cultivars characterized by a high content of tannins and high antioxidant capacity were selected. [ABSTRACT FROM AUTHOR]

Abstract Samryeongbaekchul-san (SBS) is a traditional herbal formula, which is used for the treatment of dyspepsia, chronic gastritis, and anorexia in Korea. To evaluate the quality of SBS decoction by quantifying its main constituents simultaneously using high-performance liquid chromatography coupled with photodiode array (HPLC–PDA) detection, and secondly to determine the antiadipogenic effect of SBS decoction. The main constituents in a 10-μL injection volume of the decoction were separated on Gemini C 18 and Luna NH 2 columns (both 250 mm × 4.6 mm, 5 μm) at 40 °C using a gradient of two mobile phases eluting at 1.0 mL/min. 3T3-L1 preadipocytes were differentiated into adipocytes for 8 days with or without SBS. After differentiation, accumulated triglyceride contents and leptin production were measured. The correlation coefficients of all constituents in a calibration curve were ≥0.9998 and showed good linearity in the tested concentration range after validation of the method established. The recovery of the four major compounds were 99.46–102.61% with intra- and interday precisions of 0.08–1.01% and 0.15–0.99%, respectively. The four compounds in the lyophilized SBS sample were detected up to 6.46 mg/g. SBS treatment of the differentiated adipocytes significantly inhibited lipid accumulation and leptin production without cytotoxicity. Optimized simultaneous determination of constituents by HPLC–PDA detection will help to improve quality assessment of SBS or related formulas. SBS has an antiadipogenic effect and further investigation to establish the mechanisms of action of its antiadipogenic effect is warranted. [ABSTRACT FROM AUTHOR]

Stone fruits, including peach (Prunus persica L.), nectarine (Prunus nucipersica L.), plum (Prunus domestica L.) and apricot (Prunus armeniaca L.) are common commercial fruits in the market. However, a huge amount of stone fruits waste is produced throughout the food supply chain during picking, handling, processing, packaging, storage, transportation, retailing and final consumption. These stone fruits waste contain high phenolic content which are the main contributors to the antioxidant potential and associated health benefits. The antioxidant results showed that plum waste contained higher concentrations of total phenolic content (TPC) (0.94 ± 0.07 mg gallic acid equivalents (GAE)/g) and total flavonoid content (TFC) (0.34 ± 0.01 mg quercetin equivalents (QE)/g), while apricot waste contained a higher concentration of total tannin content (TTC) (0.19 ± 0.03 mg catechin equivalents (CE)/g) and DPPH activity (1.47 ± 0.12 mg ascorbic acid equivalents (AAE)/g). However, nectarine waste had higher antioxidant capacity in ferric reducing-antioxidant power (FRAP) (0.98 ± 0.02 mg AAE/g) and total antioxidant capacity (TAC) (0.91 ± 0.09 mg AAE/g) assays, while peach waste showed higher antioxidant capacity in 2,2′-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS) assay (0.43 ± 0.09 mg AAE/g) as compared to other stone fruits waste. Qualitative and quantitative phenolic analysis of Australian grown stone fruits waste were conducted by liquid chromatography coupled with electrospray-ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS/MS) and HPLC-photodiode array detection (PDA). The LC-ESI-QTOF-MS/MS result indicates that 59 phenolic compounds were tentatively characterized in peach (33 compounds), nectarine (28), plum (38) and apricot (23). The HPLC-PDA indicated that p-hydroxybenzoic acid (18.64 ± 1.30 mg/g) was detected to be the most dominant phenolic acid and quercetin (19.68 ± 1.38 mg/g) was the most significant flavonoid in stone fruits waste. Hence, it could be concluded that stone fruit waste contains various phenolic compounds and have antioxidant potential. The results could support the applications of these stone fruit wastes in other food, feed, nutraceutical and pharmaceutical industries.

Pear (Pyrus communis L.) is widely spread throughout the temperate regions of the world, such as China, America and Australia. This fruit is popular among consumers due to its excellent taste and perceived health benefits. Various bioactive compounds, which contribute to these health benefits, have been detected in the pear fruits, including a range of phenolic compounds. Five Australian grown pear varieties, which include Packham’s Triumph, Josephine de Malines, Beurre Bosc, Winter Nelis and Rico were selected for this study to examine the phenolic compounds in pears. Beurre Bosc exhibited the highest total polyphenol content (TPC) (3.14 ± 0.02 mg GAE/g), total tannin content (TTC) (1.43 ± 0.04 mg CE/g) and 2,2′-diphenyl-1-picrylhydrazyl (DPPH) (5.72 ± 0.11 mg AAE/g), while the Josephine de Malines variety was high in total flavonoid content (TFC) (1.53 ± 0.09 mg QE/g), ferric reducing antioxidant power (FRAP) (4.37 ± 0.04 mg AAE/g), 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) (4.44 ± 0.01 mg AAE/g) and total antioxidant capacity (TAC) (5.29 ± 0.09 mg AAE/g). The liquid chromatography coupled with electrospray-ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS/MS) data indicate that a total of 73 phenolic compounds were detected in Beurre Bosc (37 compounds), Josephine de Malines (34), Rico (22), Packham’s Triumph (15) and Winter Nelis (9), respectively. From HPLC-PDA quantification, the Beurre Bosc pear variety showed significantly higher in phenolic acids (chlorogenic acid; 17.58 ± 0.88 mg/g) and while flavonoids were significantly higher in Josephine de Malines (catechin; 17.45 ± 1.39 mg/g), as compared to other pear varieties. The analyses suggest that the Australian grown pears might contain an ideal source of phenolic compounds which benefit human health. The information provided by the present work can serve as practical supporting data for the use of pears in the nutraceutical, pharmaceutical and food industries.

The increased risk of illness and disability is related to the age inevitable biological changes. Oxidative stress is a proposed mechanism for many age-related diseases. The crucial importance of polyphenol pharmacophore for aging process is largely described thanks to its effects on concentrations of reactive oxygen species. Resveratrol (3,5,4′-trihydroxy-trans-stilbene, RSV) plays a critical role in slowing the aging process but has a poor bioavailabity after oral intake. In this present work, a series of RSV derivatives was designed, synthesized, and evaluated as potential antioxidant agents. These derivatives contain substituents with different electronic and steric properties in different positions of aromatic rings. This kind of substituents affects the activity and the bioavailability of these compounds compared with RSV used as reference compound. Studies of Log P values demonstrated that the introduction of halogens gives the optimum lipophilicity to be considered promising active agents. Among them, compound 6 showed the higher antioxidant activity than RSV. The presence of trifluoromethyl group together with a chlorine atom increased the antioxidant activity compared to RSV.

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. 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. 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 (IC 50 < 100 μg/ml) potential in DPPH assay. Moreover, these floral MetOH and DCM extracts were found to be most active (>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 IC 50 < 150 μg/ml against P. aeruginosa MDR and S. aureus MDR better than moxifloxacin and was further confirmed by light and scanning electron microscopy. Moreover, the floral-MetOH extract of N. procumbens has been found to be safe up to 2 g/kg BW with its lethal dose (LD 50) as 3872.98 mg/kg BW in rats. Hence, due to presence of essential medicinal compounds with low toxicity effects, the plant is recommended to be safely employed in various pharmaceutical preparations. [ABSTRACT FROM AUTHOR]

• Determination of ABM, IVM, ABZ and its metabolites in meat by HPLC-PDA. • This method shows a reduced detection time and can be used with more targets. • The process of the chromatography conditions is optimized. Antimicrobial drugs are frequently used in a combination or shuttle way to cope with coinfection of bacteria or parasites and prevent drug resistance, thus the accurate quantification of multiple drug residues in animal-derived foods is crucial to ensure food safety. Here, a simple and efficient high-performance liquid chromatography-photodiode array (HPLC-PDA) method was established for the simultaneous quantitative screening of six common residues of antiparasitic drugs, including abamectin (ABM), ivermectin (IVM), albendazole (ABZ) and the three metabolites of ABZ in beef and chicken. The LODs and LOQs for six target compounds in beef and chicken are determined to be 3.2 to 12.5 µg/kg and 9.0 to 30.0 µg/kg, respectively. The calibration curves show good linearity (R2 ≥ 0.9990) between the peak area and concentration. The recoveries from the fortified blank samples are all above 85.10%. Finally, the applicability of the HPLC-PDA method is successfully demonstrated by the real sample analysis. [ABSTRACT FROM AUTHOR]

The poly prescription and co-administration of more than two drugs to treat patients for the disease conditions are inexorable. Heparin is an anticoagulant often administered with fenofibric acid in cardiac treatments. A reverse phased high-performance liquid chromatography method based on photo diode array detection has been developed for their simultaneous determination from admixture. They were separated using potassium dihydrogen orthophosphate: acetonitrile (20:80, V/V), on C18 column, at a flow rate of 0.8 mL/min. The retention time of heparin and fenofibric acid was 3.8 and 13.1 min, respectively. The validation parameters were studied as per ICH guidelines to ascertain the validity of the method for the purpose intended. The linearity was observed between 0.5-3 I.U./mL of heparin and 0.25-1.5 pg/mL of fenofibric acid. The method was applied to a synthetically prepared admixture, and found to be satisfactorily resolving two drugs without any interference, with good precision and reproducibility in the established condition. [ABSTRACT FROM AUTHOR]

Haedoksamul-tang (HST) is a traditional medical prescription comprising eight medicinal herbs: Angelica gigas, Cnidium officinale, Coptis japonica, Gardenia jasminoides, Paeonia lactiflora, Phellodendron amurense, Rehmannia glutinosa, and Scutellaria baicalensis. HST is used to treat blood circulation disorders and has anti-inflammatory, hemostatic, and anticonvulsant effects. In this study, a high-performance liquid chromatography/photodiode array detector (HPLC–PDA) method was developed and validated for the simultaneous determination of four marker compounds in HST, namely, berberine, palmatine, geniposide, and paeoniflorin. Four standard solutions and HST sample solutions were analyzed using a reverse-phase SunFire®C18 column (4.6 × 250 mm, 5 μm) using a 0.05% aqueous formic acid/methanol gradient. The column temperature, flow rate, injection volume, and wavelengths used were 28 ± 2 ℃, 1.0 mL/min, 10.0 μL, and 230 nm and 240 nm, respectively. Calibration curves of the four marker compounds showed good linearity (r2 ≥ 0.9994), and limits of detection (LODs) and quantification (LOQs) were in the ranges 0.131–0.296 μg/mL and 0.398–0.898 μg/mL, respectively. Ranges of intra- and inter-day precisions and accuracies values were 96.74–102.53% and 97.95–100.83%, respectively, and relative standard deviation (RSD) values were all

Haepyoyijin-tang (HPYJT) is a traditional herbal prescription that is composed of 12 medicinal herbs. Although HPYJT is frequently used in patients with asthma in Korea, no quality assessment protocols have been developed. In the present study, qualitative and quantitative analyses were performed using high-performance liquid chromatography and liquid chromatography–tandem mass spectrometry on the eight main components (mulberroside A, amygalin, liquiritin apioside, liquiritin, narirutin, hesperidin, rosmarinic acid, and glycyrrhizinic acid) to establish a quality control protocol for HPYJT. The simultaneous analysis method developed was satisfactorily validated with respect to linearity, limit of detection, limit of quantification, recovery, and precision. This analytical method thus provides an efficient approach for the evaluation of HPYJT quality.

Seaweed is an important food widely consumed in Asian countries. Seaweed has a diverse array of bioactive compounds, including dietary fiber, carbohydrate, protein, fatty acid, minerals and polyphenols, which contribute to the health benefits and commercial value of seaweed. Nevertheless, detailed information on polyphenol content in seaweeds is still limited. Therefore, the present work aimed to investigate the phenolic compounds present in eight seaweeds [Chlorophyta (green), Ulva sp., Caulerpa sp. and Codium sp.; Rhodophyta (red), Dasya sp., Grateloupia sp. and Centroceras sp.; Ochrophyta (brown), Ecklonia sp., Sargassum sp.], using liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS/MS). The total phenolic content (TPC), total flavonoid content (TFC) and total tannin content (TTC) were determined. The antioxidant potential of seaweed was assessed using a 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay, a 2,2′-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) free radical scavenging assay and a ferric reducing antioxidant power (FRAP) assay. Brown seaweed species showed the highest total polyphenol content, which correlated with the highest antioxidant potential. The LC-ESI-QTOF-MS/MS tentatively identified a total of 54 phenolic compounds present in the eight seaweeds. The largest number of phenolic compounds were present in Centroceras sp. followed by Ecklonia sp. and Caulerpa sp. Using high-performance liquid chromatography-photodiode array (HPLC-PDA) quantification, the most abundant phenolic compound was p-hydroxybenzoic acid, present in Ulva sp. at 846.083 ± 0.02 μg/g fresh weight. The results obtained indicate the importance of seaweed as a promising source of polyphenols with antioxidant properties, consistent with the health potential of seaweed in food, pharmaceutical and nutraceutical applications.

Sojadodamgangki-tang (SDGT) is a traditional Korean medicine consisting of 12 medicinal herbs that has been used in Korea for the treatment of asthma since ancient times. However, the quality control of herbal formulas that contain two or more herbal medicines remains challenging. In this study, 14 marker components were analyzed simultaneously by using high-performance liquid chromatography with photodiode array detection in addition to the use of liquid chromatography–tandem mass spectrometry for quality evaluation of SDGT. The simultaneous determination of the 14 marker components was validated in terms of linearity, recovery, and precision. The established methods can provide useful data for the quality control of SDGT and related herbal formulas.

Yeonkyopaedok-san is a traditional Korean medicine used in the early treatment of boils. In the present study, its 12 marker components for quality control were determined using high-performance liquid chromatography (HPLC) with photodiode array detection and ultra-performance liquid chromatography−mass spectrometry with tandem mass spectrometry (UPLC−MS/MS). The investigated 12 marker components of Yeonkyopaedok-san were as follows: 3-caffeoylquinic acid, cimifugin 7-glucoside, liquiritin apioside, ferulic acid, narirutin, 5-O-methylvisammioside, naringin, neohesperidin, oxypeucedanin hydrate, arctigenin, glycyrrhizic acid, and 6-gingerol. The analytical column used for the separation of the 12 marker analytes in Yeonkyopaedok-san was a Waters SunFire C18 column (4.6 mm × 250 mm, 5 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and 0.1% (v/v) formic acid in acetonitrile. In the UPLC−MS/MS analysis, all components were separated using a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and acetonitrile. The coefficient of determination of the calibration curves in both analysis systems showed good linearity (>0.99). The amounts of the 12 marker components in Yeonkyopaedok-san determined using HPLC−photodiode array detection and UPLC−MS/MS analyses were found to be 0.14−9.00 mg/g and 2.35−853.11 μg/g, respectively.

Cotoneaster plants are sources of traditional medicines and dietary products, with health benefits resulting from their phenolic contents and antioxidant activity. In this work, active markers of the leaves of C. bullatus and C. zabelii were characterized and evaluated in an integrated phytochemical and biological activity study. Based on UHPLC-PDA-ESI-MS3 analysis, twelve analytes were preselected from the constituents of the hydromethanolic leaf extracts, and two of them—caffeoylmalic acid and quercetin 3--O-β-d-(2″--O-β-d-xylopyranosyl)galactopyranoside (QPH)—were isolated for full identification (NMR spectroscopy: 1H, 13C, COSY, HMBC, HMQC). All selected phenolics contributed to the antioxidant activity of the extracts, which was demonstrated in chemical in vitro tests (DPPH, FRAP, and TBARS) and in a biological model of human plasma exposed to oxidative/nitrative stress induced by peroxynitrite. This contribution was partly due to the synergy between individual polyphenols, evidenced by an isobolographic analysis of the interactions of (−)-epicatechin, chlorogenic acid, and QPH as representatives of three classes of Cotoneaster polyphenols. All twelve markers, including also neochlorogenic acid, cryptochlorogenic acid, procyanidin B2, procyanidin C1, rutin, hyperoside, isoquercitrin, and quercitrin, were thus applied as calibration standards, and a fast, accurate, reproducible, and fully validated RP-HPLC-PDA method for quality control and standardization of the target extracts was proposed.

A reversed-phase liquid chromatographic method was developed for the assay of synephrine in Citrus aurantium dry extract. The chromatographic separation used a C18 (250 × 4.6 mm, 5 µm) column and a mobile phase consisting of acetonitrile: 0.01% orthophosphoric acid (pH 3.0) at a 15:85 ratio, flow rate of 1 mL min-1 and detection at 220 nm. The detector response was linear in the range 15 - 45 mg mL-1. Specificity and stability, indicating suitability of the method, were confirmed using stress conditions (acid and basic hydrolysis, oxidation and photolysis). Intraday precision yielded RSD values of less than 1.77% and interday precision of 2.5%. The average recovery accuracy of the test was 102.03%. The method was validated according to international guidelines and can be used in routine quality control and stability studies of Citrus aurantium preparations. The preliminary stability study showed that synephrine is susceptible to hydrolysis, oxidation and photolysis.

Dry leaf extracts of eastern teaberry (Gaultheria procumbens L.) were evaluated as a source of bioactive phytocompounds through systematic activity testing and phytochemical profiling. The antioxidant efficiency was tested using five complementary in vitro models (DPPH; FRAP; linoleic acid (LA) peroxidation assay; O2•− and H2O2 scavenging tests) in parallel with standard antioxidants. The 75% methanol extract and its diethyl ether, ethyl acetate (EAF), n-butanol and water fractions exhibited the dose-dependent responses in all assays, with the highest capacities found for EAF (DPPH EC50 = 2.9 μg/mL; FRAP = 12.8 mmol Fe2+/g; IC50 for LA-peroxidation = 123.9 μg/mL; O2•− SC50 = 3.9 μg/mL; H2O2 SC50 = 7.2 μg/mL). The EAF had also the highest anti-inflammatory activity in the inhibition tests of lipoxygenase and hyaluronidase (60.14% and 21.83% effects, respectively, at the concentration of 100 μg/mL). Activity parameters of the extracts correlated strongly with the levels of total phenolics (72.4–270.7 mg GAE/g), procyanidins, and phenolic acids, whereas for flavonoids only moderate effects were observed. Comprehensive UHPLC-PDA-ESI-MS3 and HPLC-PDA studies led to the identification of 35 polyphenols with a procyanidin A-type trimer, quercetin 3-O-glucuronide, isomers of caffeoylquinic acids, and (‒)-epicatechin being the dominant components. Significant activity levels, high phenolic contents and high extraction yields (39.4%–42.5% DW for defatted and crude methanol extracts, respectively) indicate the value of eastern teaberry leaves as bioactive products.

Graphical abstract Highlights • Three extracts of two Broccoli species was investigated for biochemical properties. • Key enzyme inhibitory effects were investigated. • We observed protective effects on bladder, kidney and liver. • Catechin, epicatechin, vanillic and 3-hydroxy benzoic acids are main compounds in the extracts. • The Broccoli species could be regarded as potential ingredients for designing novel functional supplements. Abstract In this study, three different extracts (soxhlet, microwave and decoction) from two species of broccoli: Brassica oleracea L. convar. Italica botrytis (L.) Alef. var. cymosa Duch. (Broccolo Fiolaro) and Brassica oleracea acephala L. convar. acephala (DC.) Alef. var. sabellica L. (Cavolo Nero), which are commonly spread in north-central Italy, were tested for their enzyme inhibitory effects. Enzyme inhibitory effects were investigated against cholinesterases, tyrosinase, α-amylase and α-glucosidase. The soxhlet extracts had the highest inhibitory AChE effects with 1.08 mgGALAE/g (in Cavolo Nero) and 0.90 mgGALAE/g (in Broccolo Fiolaro). The significant tyrosinase inhibitory effect was observed in the soxhlet extract of Cavolo Nero with 11.93 mgKAE/g. In addition, we evaluated the antioxidant activity of Broccolo Fiolaro and Cavolo Nero on lipopolysaccharide (LPS)-stimulated bladder, kidney and liver specimens, ex vivo. We observed a significant reduction of both nitrite and malondialdehyde (MDA) following treatment that indicates a significant inhibitory effect on oxidative/nitrosative stress and lipoperoxidation, respectively. Additionally, the blunting effect induced by extracts on LPS-induced lactate dehydrogenase (LDH) activity further support a protective effect by both Broccolo Fiolaro and Cavolo Nero in bladder, kidney and liver. HPLC analysis revealed that catechin, epicatechin, vanillic and 3-hydroxy benzoic acids were the major components. The phenolic components may contribute to the observed enzyme inhibitory effects. in vivo tests also demonstrated that the extracts decreased the biochemical parameters in diabetic rats. Particularly, we observed the reduction of plasma glucose levels, urea and total cholesterol following oral administration, with the higher inhibitory effects exerted by Broccolo Fiolaro compared to Cavolo Nero. Overall, our results could provide new insights on the use of these Broccoli species not only as foods but also as functional and nutraceutical supplements. [ABSTRACT FROM AUTHOR]

Trillium govanianum Wall. ex D. Don (Melanthiaceae alt. Trilliaceae), commonly known as ‘nagchhatry’ or ‘teen patra’, distributed from Pakistan to Bhutan about 2500-3800 m altitude is indigenous to Himalayas region. In folk medicine the plant has been reported for the treatment of wound healing, sepsis and in various sexual disorders. This paper reports, for the first time, to evaluate the cytotoxicity, in vitro anti-leishmanial (promastigotes) and fingerprint HPLC-photodiode array analysis of the MeOH extract of the roots of T. govanianum and its solid phase extraction fractions. Reverse phase HPLC-PDA based quantification revealed the presence of significant amount of quercetin, myrecetin and kaemferol ranging from 0.221to 0.528 μg/mg DW. MeOH extract revealed distinguishable protein kinase inhibitory activity against Streptomyces 85E strain with 18 mm bald phenotype. The remarkable toxicity profile against brine shrimps and leishmanial was manifested by MeOH extract with LC50 10 and 38.5 μg/mL, respectively. [ABSTRACT FROM AUTHOR]

A rapid and simple high-performance liquid chromatography method with a Photo Diode Array (PDA) detector is developed for the simultaneous analysis of seven kaempferol, quercetin and myricetin derivatives along with an acylated flavonoid glycoside; trans-tiliroside from different Cistus species. In this study, the qualitative and quantitative analysis of the methanolic extracts of three Cistus species (C. creticus L., C. laurifolius L. and C. salviifolius L.) growing in Anatolia in terms of characterization of flavonoid compounds were performed by RP-HPLC for the first time. Trans-tiliroside, a mono-coumaroyl kaempferol glucoside was found to be the most abundant flavonoid in C. salviifolius (0.276±0.003 g/100 gextract) and C. creticus (0.253±0.001 g/100 gextract) while hyperin (0.149±0.004 g/100 gextract) and myricetin 3-O-β-galactopyranoside (0.139±0.006 g/100 gextract) were found to be the most intense flavonoids in C. laurifolius samples. The described HPLC method appears suitable for the determination of the Cistus flavonols and their glycosides and can be considered as an effective and alternative procedure for the identification and quantification of this important class of biologically active compounds. [ABSTRACT FROM AUTHOR]

In the present work, fourteen cultivars of Prunus domestica were analyzed to investigate their phenolic pattern with the purpose of using the leaves as potential resources of bioactive compounds in the pharmaceutical and food industry. Microwave-assisted extraction (MAE), dispersive liquid–liquid microextraction and sugaring-out liquid–liquid extraction techniques were optimized in order to obtain an exhaustive multi-component panel of phenolic compounds. The best phenolic-enriched recovery was achieved using MAE in water:methanol (30:70), and this procedure was further applied for quantitative analysis of phenolic compounds in real samples. In order to prove the safeness of these extracts, the biological potential of the Prunus cultivars was tested by several in vitro antioxidant and enzyme inhibitory assays. Moreover, their cytotoxicity was evaluated on human gingival fibroblasts (HGFs), and in most of the cases the treatment with different concentrations of extracts didn't show cytotoxicity up to 500 μg/mL. Only ‘Carpatin’ and ‘Minerva’ cultivars, at 250 and 500 μg/mL, reduced partially cell viability of HGFs population. Noteworthy, Centenar cultivar was the most active for the α-glucosidase inhibition (6.77 mmolACAE/g extract), whereas Ialomița cultivar showed the best antityrosinase activity (23.07 mgKAE/g extract). Overall, leaves of P. domestica represent a rich alternative source of bioactive compounds. [ABSTRACT FROM AUTHOR]

In the present work, antioxidant compounds from Teucrium montanum were extracted by subcritical water. The influence of extraction temperature and pressure on antioxidant activity of extracts has been investigated in terms of extraction yield (EY), total phenolic content (TPC), and DPPH-radical scavenging activity (DPPH-RSA) and ferric reducing antioxidant power (FRAP). Additionally, the compounds responsible for the antioxidant activity were identified and quantified by high performance liquid chromatography (HPLC). The highest EY (42.63%), TPC (174.61 ± 4.09 mg GAE/g DE) and antioxidant activity by DPPH-RSA (176.23 ± 8.76 mg TE/g DE) and FRAP (141.71 ± 5.21 mg AAE/g DE) were seen in extracts obtained at temperature of 160 °C and pressure of 10 bar. HPLC analysis revealed that naringin and gallic acid were the principle antioxidant compounds in subcritical extracts. According to the results, SWE has a great potential in exploitation of natural sources of bioactive compounds and production of pharmacologically-active fractions. [ABSTRACT FROM AUTHOR]