STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF SIMETHICONE, DOMPERIDONE, MAGALDRATE AND SODIUM ALGINATE: APPLICATION TO SYRUP FORMULATION

A rapid and validated stability indicating RP-HPLC method using isocratic elution and coupled with photodiode array detection was developed for quantifying the content of simethicone, domperidone, magaldrate and sodium alginate in bulk and syrup formulation. The best mobile phase used in this study consisted of 0.1 % orthophosphoric acid/acetonitrile (50/50, V/V) with a flow rate of 0.7 mL min-1. Under optimized conditions used in this study, selected drugs were eluted at 3.301 min (simethicone), 4.293 min (domperidone), 5.220 min (magaldrate) and 6.149 min (sodium alginate) within 12 min run time without any interfering excipients. Peak areas and selected drug content demonstrated excellent linearity (simethicone – 5 to 30 µg mL-1; domiperidone – 2.5 to 15 µg mL-1; magaldrate – 120 to 720 µg mL-1; sodium alginate – 25 to 150 µg mL-1). Percent recovery, which represents accuracy, was 99.12–100.18 % for simethicone, 99.59-100.52 % for domperidone, 99.23-100.25 % for magaldrate and 99.57-100.02 % for sodium alginate. Percent relative standard deviation, which represents precision, was observed in the range of 0.078-0.983 % (simethicone), 0.528-0.861 % (domperidone), 0.278-1.069 % (magaldrate), 0.316-0.572 % (sodium alginate). The developed method displayed favourable accuracy and recovery and was suitable for determining the content of simethicone, domperidone, magaldrate and sodium alginate combination in syrup formulations.

Is Our Natural Food Our Homeostasis? Array of a Thousand Effect-Directed Profiles of 68 Herbs and Spices

The beneficial effects of plant-rich diets and traditional medicines are increasingly recognized in the treatment of civilization diseases due to the abundance and diversity of bioactive substances therein. However, the important active portion of natural food or plant-based medicine is presently not under control. Hence, a paradigm shift from quality control based on marker compounds to effect-directed profiling is postulated. We investigated 68 powdered plant extracts (botanicals) which are added to food products in food industry. Among them are many plants that are used as traditional medicines, herbs and spices. A generic strategy was developed to evaluate the bioactivity profile of each botanical as completely as possible and to straightforwardly assign the most potent bioactive compounds. It is an 8-dimensional hyphenation of normal-phase high-performance thin-layer chromatography with multi-imaging by ultraviolet, visible and fluorescence light detection as well as effect-directed assay and heart-cut of the bioactive zone to orthogonal reversed-phase high-performance liquid chromato-graphy−photodiode array detection−heated electrospray ionization mass spectrometry. In the non-target, effect-directed screening via 16 different on-surface assays, we tentatively assigned more than 60 important bioactive compounds in the studied botanicals. These were antibacterials, estrogens, antiestrogens, androgens, and antiandrogens, as well as acetylcholinesterase, butyrylcholinesterase, α-amylase, α-glucosidase, β-glucosidase, β-glucuronidase, and tyrosinase inhibitors, which were on-surface heart-cut eluted from the bioautogram or enzyme inhibition autogram to the next dimension for further targeted characterization. This biological-physicochemical hyphenation is able to detect and control active mechanisms of traditional medicines or botanicals as well as the essentials of plant-based food. The array of 1,292 profiles (68 samples × 19 detections) showed the versatile bioactivity potential of natural food. It reveals how efficiently and powerful our natural food contributes to our homeostasis.

Mobility of Organotin Pesticides: Azocyclotin And Cyhexatin In Clayey And Sandy Soils From The Northern Paraná State - Brazil

Azocyclotin and cyhexatin are pesticides commonly used in mite control. However, these organotin compounds are highly harmful to the aquatic ecosystem and supposedly mobile in the soil. In addition to not existing defined rules of use, few studies have been carried out on organotins' behavior and environmental control. Liquid chromatography has been pointed out for the OTC quantitation because of gas chromatography's thermal stability and derivatization limitations. Hence, a new high-performance liquid chromatography method with photodiode array detection (HPLC-PDA) was developed for quality assurance and quality control (QA/QC) and environmental performance assessment purposes. Hysteresis index (\emph{HI}) and mobilization factor were determined from sorption/desorption in sandy and clayey soils to assess mobility and environmental risk. Mobilization was observed for the two compounds by applying the dual-mode Freundlich-Langmuir model to the isotherms. Azocyclotin showed greater mobility, 23\% and 19\%, and \emph{HI} of $-$0.15 and 7.8$\times$10$^{-4}$ for clayey and sandy soil samples, respectively. Although cyhexatin was practically immobile for both soil samples, it can be mobilized as an azocyclotin metabolite, increasing the environmental impact and risk for agricultural uses.

Phytohormones and Elicitors Enhanced the Ecdysteroid and Glycosylflavone Content and Antioxidant Activity of Silene repens

In the course of the ongoing chemical study of species of Silene genus, S. repens Patrin as a common species of the genus, was selected as the object of this study. Using high-performance liquid chromatography with photodiode array detection and electrospray ionization triple quadrupole mass spectrometric detection (HPLC-PDA-ESI-tQ-MS), the presence of 12 ecdysteroids and 6 glycosylflavones was established in S. repens introduced seedlings. 20-Hydroxyecdysone and polypodine B, as well as sileneside E and schaftoside, were the dominant compounds in introduced seedlings of S. repens. The effect of exogenous phytohormones and elicitors on the productivity and accumulation of ecdysteroids and glycosylflavones in introduced seedlings of S. repens was investigated for the first time. It was found that the use of ethyl arachidonate (100 mg/L) to increase the productivity of S. repens is justified. To obtain S. repens with a high content of ecdysteroids and glycosylflavones, it is recommended to apply epibrassinolide (100 mg/L) and 4-chlorophenoxyacetic acid (100 mg/L), respectively. Antioxidant activity of S. repens against 2,2-diphenyl-1-picrylhydrazyl radical (DPPH·) was determined, and it was revealed that sileneside E and schaftoside, as well as meloside А and isovitexin had the highest antioxidant activity among the studied compounds of S. repens.

Metabolites of Prickly Rose: Chemodiversity and Digestive-Enzyme-Inhibiting Potential of Rosa acicularis and the Main Ellagitannin Rugosin D

Prickly rose (Rosa acicularis Lindl.) is the most distributed rose species in the Northern Hemisphere, used by indigenous people for various food purposes. The lack of detailed information about the chemical composition of R. acicularis has led us to study the phytochemical composition and metabolic profile of prickly rose extracts using chromatographic techniques. Many groups of phenolic and non-phenolic compounds were quantified in the leaves, flowers, roots and fruits of R. acicularis. Phenolic compounds were the dominant phytochemicals in the aerial parts and roots of R. acicularis. A precise study by high-performance liquid chromatography with photodiode array detection and electrospray ionization triple quadrupole mass spectrometric detection showed the presence of 123 compounds, among which ellagic acid derivatives, ellagitannins, gallotannins, catechins, catechin oligomers, hydroxycinnamates and flavonoid glycosides of kaempferol, quercetin and dihydroquercetin were all identified for the first time. The most abundant phenolic compounds were ellagitannins and flavonoid glycosides, with a maximal content of 70.04 mg/g in leaves and 66.72 mg/g in flowers, respectively, indicating the great ability of R. acicularis organs to accumulate phenolic compounds. By applying a standardized static, simulated gastrointestinal digestion method, we found the inhibitory potential of the leaf extract against digestive α-amylases. A pancreatic α-amylase activity-inhibiting assay coupled with HPLC microfractionation demonstrated high inhibition of enzyme activity by ellagitannin rugosin D, which was later confirmed by a microplate reaction with mammalian α-amylases and the simulated digestion method. This study clearly demonstrates that R. acicularis leaf extract and its main component, ellagitannin rugosin D, strongly inhibit digestive α-amylase, and may be a prospective antidiabetic agent.

Association of Plasma Carotenoid and Malondialdehyde Levels with Physical Performance in Korean Adolescents

Background Increased oxidative stress has been shown to lead to muscle damage and reduced physical performance. The antioxidant mechanism is most likely to reduce these relationships, but in the context of the action of carotenoids, more research is needed. This cross-sectional study aims to investigate whether carotenoids modify the association between plasma malondialdehyde (MDA) and physical performance in Korean adolescents. Methods The study sample consisted of 381 participants (164 boys, 217 girls) aged 13−18, who participated in the 2018 National Fitness Award Project. We quantified α-carotene, β-carotene, β-cryptoxanthin, lutein, zeaxanthin, lycopene, and MDA levels in plasma using HPLC with photodiode array detection. Physical performance was measured by determining the absolute and relative hand grip strength, 20-m progressive aerobic cardiovascular endurance run, estimated maximal oxygen consumption, curl-up, and sit-and-reach. Results In boys, the multiple linear regression model adjusted for age, BMI, smoking, drinking, and physical activity showed that the MDA level was negatively associated with absolute hand grip strength; this association was observed only in groups with α-carotene, β-cryptoxanthin, zeaxanthin, and total carotenoid values below the median. Conclusion These results suggest that carotenoids may act as an effect modifier of the association between MDA and physical performance in Korean male adolescents.

Potential Activity of Abrantes Pollen Extract: Biochemical and Cellular Model Studies

The aim of this study was to determine the grain composition and (poly)phenolic profile of pollen from Abrantes (Portugal), as well as its antioxidative and antidiabetic properties, and abilities to protect human erythrocytes against induced hemoglobin oxidation, lipid peroxidation, and hemolysis. The phytochemical profile of the Abrantes’ bee pollen revealed twenty phenolic compounds, identified by high-performance liquid chromatography with electrospray ionization mass spectrometry coupled with photodiode array detection. Among them, quercetin derivatives were the most abundant. Concerning the biological potential, the pollen extract showed notable capacity for 2,2-diphenyl-1-picrylhydrazyl, nitric oxide, and superoxide radicals, as well as for inhibition of α-glucosidase action, and protection of human erythrocytes against oxidative damage. Non-cytotoxic effects regarding the NHDF normal cell line, human adenocarcinoma Caco-2, and human liver HepG2 cells were observed. The results obtained contributed to further research on modes of action related to oxidative damage and metabolic health problems, to generate deeper knowledge of potential health-promoting effects to develop novel pharmaceutical drugs, nutraceuticals, and dietary supplements.

Development and Validation of a Stability-Indicating HPLC Method for the Simultaneous Determination of trans-Resveratrol and cis-Resveratrol in an Injectable Solution

trans-Resveratrol, a phytochemical compound with antioxidant power and various therapeutic effects, such as cardioprotective, chemopreventive, and neuroprotective, among others, has disadvantages of poor solubility and limited stability, creating difficulties for the development of new strategies for its quantification. This study developed and validated an analytical stability method for trans-resveratrol by high-pressure liquid chromatography with photodiode-array detection (HPLC-PDA), which allowed its quantification in the presence of its degradation products. The quantification of trans-resveratrol occurred at a retention time of 2.6 min, with ammonium formate (10 mM, pH = 4)/acetonitrile, 70/30 v/v, as mobile phase. The validation met the ICH Q2 criteria of specificity, method linearity (2.8–4.2 μg/ml), precision and accuracy, robustness, quantification limit (0.176 μg/ml), and detection (0.058 μg/ml). As degradation products, cis-resveratrol was observed at 3.9 min, which could be resveratrone in 3.2 min and five unidentified products in 0.7, 1.0, 1.4, 1.8, and 5 min. Some solutions subjected to temperature stress of 40 and 60°C, UV light, and acidic and basic hydrolysis exhibited colour changes. An analytical method was obtained by HPLC-PDA, which allowed quantifying the stability of trans-resveratrol in a fast and specific manner in the presence of its degradation products.

LC-MS/MS-QTOF Screening and Identification of Phenolic Compounds from Australian Grown Herbs and Their Antioxidant Potential

Culinary spices and herbs have been used to impart a characteristic flavour and aroma in food due to their appealing fragrance. Recently, bioactive compounds from herbs, especially phenolics, have gained much attention due to their potential health outcomes. The aim of this study was to characterize and quantify the phenolic compounds from 10 widely used Australian-grown herbs (oregano, rosemary, bay, basil, sage, fenugreek, dill, parsley, mint and thyme). For this purpose, liquid chromatography mass spectrometry (LC-MS) was used for the complete profiling of polyphenolic compounds and quantification of abundant phenolic compounds was completed with high-performance liquid chromatography—photodiode array detection (HPLC-PDA). Polyphenols from Australian-grown herbs were estimated through total phenolic content (TP), total flavonoids (TF) and total tannins (TT) along with their in-vitro antioxidant activities. Oregano and mint were estimated with the highest value of TP (140.59 ± 9.52 and 103.28 ± 8.08 mg GAE/g, milligram gallic acid equivalent/gram) while rosemary and mint had the highest TF (8.19 ± 0.74 and 7.05 ± 0.43 mg QE (quercetin equivalent)/g). In this study, eighty-four (84) phenolic compounds were screened and confirmed through LC-MS/MS by comparing their masses and fragmentation pattern with published libraries. The results of this study validate the use of these herbs as bioactives and their positive impact on human health.

Growth and Carotenoid Contents of Intercropped Vegetables in Building-Integrated Urban Agriculture

Sustainable food security due to climate and social change is more important than ever. This study was conducted to increase plant growth and bioactive contents using intercropping technology in urban agriculture. Tomatoes (Solanum lycopersicum L.) and sunflowers (Helianthus annuus L.) were intercropped in different ratios in outdoor rooftop, and lettuce (Lactuca savita L.) was grown with chicory (Cichorium intybus. L.) in the indoor LED plant growth chambers. Carotenoids in plant foods were analyzed using an ultraperformance liquid chromatography with photodiode array detection. Chlorophyll contents were determined by the soil analysis development chlorophyll meter. Tomatoes planted with sunflowers (3 : 1) had a significantly larger stem diameter ( p < 0.05 ), a large number of leaves ( p < 0.05 ), and significantly higher lycopene at d88 ( p < 0.05 ), d102 ( p < 0.001 ), and d115 ( p < 0.01 ), and β-carotene contents at d102 ( p < 0.05 ) as compared to those of monocultured tomatoes. Lettuce planted in a ratio of 1 : 3 with lettuce and chicory had significantly higher contents of chlorophyll ( p < 0.05 ), β-carotene ( p < 0.05 ), and lutein ( p < 0.01 ), than lettuce planted alone. On the other hand, intercropping of chicory and lettuce did not have a beneficial effect on the growth and carotenoid content of chicory. The current study indicates that plant growth and carotenoid content can be substantially modified by cocultivation, and the effects may vary depending on the type of plant and the crop ratio.