Comparison of autoclaving and γ-radiation impact on four spices aroma profiles and microbial load using HS-SPME GC-MS and chemometric tools.

Herbal spices are widely consumed as food additives owing to their distinct aroma and taste as well as a myriad of economic and health value. The aroma profile of four major spices including bay leaf, black pepper, capsicum, and fennel was tested using HS-SPME/GC-MS and in response to the most widely used spices´ processing methods including autoclaving and γ-radiation at low and high doses. Additionally, the impact of processing on microbial contamination of spices was tested using total aerobic count. GC-MS analysis led to the identification of 22 volatiles in bay leaf, 34 in black pepper, 23 in capsicum, and 24 in fennel. All the identified volatiles belonged to oxides/phenols/ethers, esters, ketones, alcohols, sesquiterpene and monoterpene hydrocarbons. Oxides/phenol/ethers were detected at high levels in all tested spices at ca. 44, 28.2, 48.8, 61.1%, in bay leaves, black pepper, capsicum, and fennel, respectively of the total blend and signifying their typical use as spices. Total oxides/phenol/ethers showed an increase in bay leaf upon exposure to γ-radiation from 44 to 47.5%, while monoterpene hydrocarbons were enriched in black pepper upon autoclaving from 11.4 in control to reach 65.9 and 82.6% for high dose and low dose of autoclaving, respectively. Cineole was detected in bay leaf at 17.9% and upon exposure to autoclaving at high dose and γ-radiation (both doses) its level increased by 29-31%. Both autoclaving and γ-radiation distinctly affected aroma profiles in examined spices. Further, volatile variations in response to processing were assessed using multivariate data analysis (MVA) revealing distinct separation between autoclaved and γ-radiated samples compared to control. Both autoclaving at 115 °C for 15 min and radiation at 10 kGy eliminated detected bioburden in all tested spices i.e., reduced the microbial counts below the detection limit (< 10 cfu/g).

Dual optical detection approach for capillary electrophoresis following two-step liquid-liquid extraction to determine ten phenols in water samples.

In this research, the analytical method was developed and evaluated for determining phenol and its nine derivatives belong to the US EPA priority pollutant list in water samples by using dual-channeled capillary electrophoresis (CE) coupled with two types of optical detectors, namely LED-induced fluorescence (LEDIF) and ultraviolet (UV) detectors. The optimal background electrolytes for the first and second CE channels were 20 mM borate (pH 9.80) with 400 µM fluorescein and 55 mM borate (pH 11.75), respectively. The two-step liquid-liquid extraction (LLE) was used for sample preparation and enrichment, in which phenol and its derivatives were extracted from the aqueous phase using 10 mL of n-hexane/1-octanol (60/40, v/v) and then were back extracted into a 0.1 M NaOH as a final acceptor phase. Under the optimal CE and two-step LLE conditions, the enrichment factors of 10 phenols were 184 - 1120-fold, and the method detection limits were lowered to 0.02-0.60 µg/L. The obtained intra-day and inter-day precisions in terms of relative standard deviations (RSD) were between 4.0 and 7.3 % and 6.7 and 14 %, respectively. This approach was used to determine phenols in water samples, with recoveries ranging from 82.0 to 108.9 %. In combination with sample enrichment by two-step LLE extraction, this is the first CE study conducted to determine phenols in the EPA list using two detector approaches, specifically CE-LEDIF/CE-UV.

Photocatalytic evaluation of synthesized MnO2/Fe3O4 NCs by Q. infectoria extract for removal Ni(II) and phenol: Study phytochemical, kinetics, thermodynamics, and antibioactivity.

In the present study, the plant extract of the Quercus infectoria galls was used as a reducing, capping, and stabilizer agent for green synthesized MnO2 nanoparticles (NPs) and MnO2/Fe3O4 nanocomposites (NCs) due to its reduction ability from polyphenol and antioxidant content. The green synthesized nanomaterials have been characterized by various techniques such as FTIR, UV-vis, XRD, SEM, EDS, and TEM. The average size of about 7.4 and 6.88 nm was estimated for the NCs crystals of SEM images and XRD analysis by the Scherrer and Williamson-Hall methods. The green synthesized MnO2/Fe3O4 NCs (dosage: 0.1 g) have shown high photocatalytic activity for the removal of Ni(II) in acidic and basic solutions under visible irradiation (220 V lamp). The removal efficiency for the Ni(II) solution (3.6 × 10-3 M) at pH = 3 was increased to pH = 12 from 56 % to 98 %. The oxidase-like activity of MnO2/Fe3O4 NCs at different dosages (0.05, 0.1, and 0.15 g) for the removal and colorimetric of phenol (1 g/40 mL) in the presence 4-AAp (1 g) was seen after only 28, 13, and 5 s, respectively. The kinetic evaluation results showed the pseudo-second-order kinetics model closely matched the adsorption capacity theoretical values qe,cal (578.03, 854.70, 892.85, and 917.43 mg.g-1) and experimental values qe,exp (521.84, 839.74, 887.86, and 913.22 mg.g-1) at different initial pH solution (3-12) for Ni(II) removal. In addition, the investigation of isotherm models revealed that the Langmuir model (R2 = 0.9955) explains a better estimate for a monolayer and favorable removal of Ni(II) ions onto NCs. Also, the low Temkin constant, BT < 0 (0.0200 kJ.mol-1), and positive ∆H° value (0.103 kJ.mol-1.K-1) illustrated that Ni(II) removal is physical sorption and endothermic process. However, the obtained thermodynamic results showed the negative values ΔG° with the increase in temperature (303-318 K) toward a spontaneous removal process of Ni(II). Finally, the plant antioxidant (200 to 3200 µg/mL) and antimicrobial activities (0.001 to 0.1 g/mL) for plant extract, MnO2 NPs, and MnO2/Fe3O4 NCs were evaluated against Gram-positive and Gram-negative bacteria species.

Interactions of legume phenols-rice protein concentrate towards improving vegan food quality: Development of a protein-phenols enriched fruit smoothie.

Phenol-protein interaction is considered an effective tool to improve the functional properties of vegan proteins. The present work aimed to evaluate the covalent interaction between kidney bean polyphenols with rice protein concentrate and studied their characteristics for quality improvement in vegan-based foods. The impact of interaction on the techno-functional properties of protein was evaluated and the nutritional composition revealed that kidney bean was rich in carbohydrates. Furthermore, a noticeable antioxidant activity (58.11 ± 1.075 %) due to the presence of phenols (5.5 mg GAE/g) was observed for the kidney bean extract. Moreover, caffeic acid and p-Coumaric acid were confirmed using ultra-pressure liquid chromatography and the amount was 194.43 and 0.9272 mg/kg, respectively. A range of rice protein- phenols complexes (PPC0.025, PPC0.050, PPC0.075, PPC0.1, PPC0.2, PPC 0.5, PPC1) were examined and PPC0.2 and PPC0.5 showed significantly (p < 0.05) higher binding efficiency with proteins via covalent interaction. The conjugation reveals changes in physicochemical properties of rice protein, including, reduced size (178.4 nm) and imparted negative charges (-19.5 mV) of the native protein. The presence of amide Ⅰ, Ⅱ, Ⅲ, was confirmed in native protein and protein-phenol complex with vibration bands, particularly at 3784.92, 1631.07, and 1234 cm-1, respectively. The X-ray diffraction pattern depicted a slight decrease in crystallinity after the complexation and scanning electron microscopy revealed the alteration in morphology from less to improved smoothness and continuous surface characteristics for the complex. Thermo gravimetric analysis revealed high thermal stability of the complex with a maximum weight loss at a temperature range of 400-500 °C. Protein-phenol complex added fruit-based smoothie was developed and it was found to be acceptable in terms of various sensory attributes including color & appearance, textural consistency, and mouthfeel as compared to the control smoothie. Overall, this study provided novel insights to understand the phenol-protein interactions and the possible use of the phenol-rice protein complex in the development of vegan-based food products.

Pollution and risk assessment of phenolic compounds in drinking water sources from South-Western Nigeria.

This study reports the occurrence and risk assessment of 2,4-dinitrophenol (2,4-DNP), phenol (PHE), and 2,4,6-trichlorophenol (2,4,6-TCP) in drinking water sources in three south-western States in Nigeria (Osun, Oyo, and Lagos). Groundwater (GW) and surface water (SW) were collected during dry and rainy seasons of a year. The detection frequency of the phenolic compounds followed the trend Phenol > 2,4-DNP > 2,4,6-TCP. The mean concentrations of 2,4-DNP, Phenol, and 2,4,6-TCP in GW/SW samples from Osun State were 639/553 µg L-1, 261/262 µg L-1, and 169/131 µg L-1 during the rainy season and 154/7 µg L-1, 78/37 µg L-1, and 123/15 µg L-1 during the dry season, respectively. In Oyo State, the mean concentrations were 165/391 µg L-1 for 2,4-DNP and 71/231 µg L-1 for Phenol in GW/SW samples, respectively, during the rainy season. Generally, in the dry season, these values decreased. In any case, these concentrations are higher than those previously reported in water from other countries. The concentration of 2,4-DNP in water posed serious ecological risks to Daphnia on the acute scale while it was algae on the chronic scale. Estimated daily intake and hazard quotient calculations suggest that 2,4-DNP and 2,4,6-TCP in water pose serious toxicity concerns to humans. Additionally, the concentration of 2,4,6-TCP in water from Osun State in both seasons of the year and in both groundwater and surface water poses significant carcinogenic risks to persons ingesting water from these sources in the State. Every exposure group studied were at risk from ingesting these phenolic compounds in water. However, this risk decreased with increasing age of the exposure group. Results from the principal component analysis indicate that 2,4-DNP in water samples is from an anthropogenic source different from that for Phenol and 2,4,6-TCP. There is a strong need to treat water from GW and SW systems in these States before ingesting while assessing their quality regularly.

Wild blueberry (poly)phenols can improve vascular function and cognitive performance in healthy older individuals: a double-blind randomized controlled trial.

BACKGROUND: Evidence suggests that the intake of blueberry (poly)phenols is associated with improvements in vascular function and cognitive performance. Whether these cognitive effects are linked to increases in cerebral and vascular blood flow or changes in the gut microbiota is currently unknown. METHODS: A double-blind, parallel randomized controlled trial was conducted in 61 healthy older individuals aged 65-80 y. Participants received either 26 g of freeze-dried wild blueberry (WBB) powder (302 mg anthocyanins) or a matched placebo (0 mg anthocyanins). Endothelial function measured by flow-mediated dilation (FMD), cognitive function, arterial stiffness, blood pressure (BP), cerebral blood flow (CBF), gut microbiome, and blood parameters were measured at baseline and 12 wk following daily consumption. Plasma and urinary (poly)phenol metabolites were analyzed using microelution solid-phase extraction coupled with liquid chromatography-mass spectrometry. RESULTS: A significant increase in FMD and reduction in 24 h ambulatory systolic BP were found in the WBB group compared with the placebo group (0.86%; 95% CI: 0.56, 1.17, P < 0.001; -3.59 mmHg; 95% CI: -6.95, -0.23, P = 0.037; respectively). Enhanced immediate recall on the auditory verbal learning task, alongside better accuracy on a task-switch task was also found following WBB treatment compared with placebo (P < 0.05). Total 24 h urinary (poly)phenol excretion increased significantly in the WBB group compared with placebo. No changes in the CBF or gut microbiota composition were found. CONCLUSIONS: Daily intake of WBB powder, equivalent to 178 g fresh weight, improves vascular and cognitive function and decreases 24 h ambulatory systolic BP in healthy older individuals. This suggests that WBB (poly)phenols may reduce future CVD risk in an older population and may improve episodic memory processes and executive functioning in older adults at risk for cognitive decline. Clinical Trial Registration number in clinicaltrials.gov: NCT04084457.

Environmental phenol exposure associates with urine metabolome alteration in young Northeast Indian females.

Urinary biomonitoring delivers the most accurate environmental phenols exposure assessment. However, environmental phenol exposure-related biomarkers are required to improve risk assessment to understand the internal processes perturbed, which may link exposure to specific health outcomes. This study aimed to investigate the association between environmental phenols exposure and the metabolome of young adult females from India. Urinary metabolomics was performed using liquid chromatography-mass spectrometry. Environmental phenols-related metabolic biomarkers were investigated by comparing the low and high exposure of environmental phenols. Seven potential biomarkers, namely histidine, cysteine-s-sulfate, 12-KETE, malonic acid, p-hydroxybenzoic acid, PE (36:2), and PS (36:0), were identified, revealing that environmental phenol exposure altered the metabolic pathways such as histidine metabolism, beta-Alanine metabolism, glycerophospholipid metabolism, and other pathways. This study also conceived an innovative strategy for the early prediction of diseases by combining urinary metabolomics with machine learning (ML) algorithms. The differential metabolites predictive accuracy by ML models was >80%. This is the first mass spectrometry-based metabolomics study on young adult females from India with environmental phenols exposure. The study is valuable in demonstrating multiple urine metabolic changes linked to environmental phenol exposure and a better understanding of the mechanisms behind environmental phenol-induced effects in young female adults.

Bio-phenols determination in olive oils: Recent mass spectrometry approaches.

Extra virgin olive oil (EVOO) is largely used in Mediterranean diet, and it is also worldwide apprised not only for its organoleptic properties but also for its healthy effects mainly attributed to the presence of several naturally occurring phenolic and polyphenolic compounds (bio-phenols). These compounds are characterized by the presence of multiple phenolic groups in more or less complex structures. Their content is fundamental in defining the healthy qualities of EVOO and consequently the analytical methods for their characterization and quantification are of current interest. Traditionally their determination has been conducted using a colorimetric assay based on the reaction of Folin-Ciocalteu (FC) reagent with the functional hydroxy groups of phenolic compounds. Identification and quantification of the bio-phenols in olive oils requires certainly more performing analytical methods. Chromatographic separation is now commonly achieved by HPLC, coupled with spectrometric devices as UV, FID, and MS. This last approach constitutes an actual cutting-edge application for bio-phenol determination in complex matrices as olive oils, mostly on the light of the development of mass analyzers and the achievement of high resolution and accurate mass measurement in more affordable instrument configurations. After a short survey of some rugged techniques used for bio-phenols determination, in this review have been described the most recent mass spectrometry-based methods, adopted for the analysis of the bio-phenols in EVOOs. In particular, the sample handling and the results of HPLC coupled with low- and high-resolution MS and MS/MS analyzers, of ion mobility mass spectrometry and ambient mass spectrometry have been reported and discussed.

Association of environmental phenols with endometriosis and uterine leiomyoma: An analysis of NHANES, 2003-2006.

Exposure to phenols is widespread since they are found in many everyday products. Given that phenols are considered endocrine disrupting chemicals with the potential to interfere with hormonal activities, they could have adverse effects on female reproductive health. We analyzed cross-sectional data from the National Health and Nutrition Examination Survey (NHANES), 2003-2006 to examine the association between phenols and endometriosis and uterine leiomyoma (fibroids). Levels of bisphenol A (BPA), benzophenone-3, and triclosan were measured using urine samples, and information on endometriosis and fibroids diagnoses as well as other relevant characteristics were ascertained using self-reported questionnaires. Multivariate logistic regression with odds ratios (ORs) and 95 % confidence intervals (CIs) were used to quantify the association between each phenol and female gynecologic condition. Our study included 700 women, of which 53 women had endometriosis and 107 women had fibroids. We found exposure to BPA to be statistically significantly positively associated with endometriosis (p = 0.05); women in the highest exposure quartile had over the three times the odds of having endometriosis relative to women in the lowest quartile (OR=3.58, 95 % CI 1.00-12.89). None of the phenols considered were significantly associated with fibroids. Overall, exposure to BPA increased the odds of having endometriosis, and there appeared to be a dose-response relationship. This suggests that BPA may play a role in the pathogenesis of endometriosis although the cross-sectional nature of NHANES data is a methodological limitation. Additional research on the impact of endocrine disrupting chemicals, like phenols, on female reproductive health should be conducted.

Comparative metabolic profiling, isolation of alkylated phenols and antioxidant activity of roots of Plumbago species using GC-MS and NMR based metabolomics study.

In this study, NMR and GC-MS based comparative metabolomic profiling of the roots of three different species namely, Plumbago indica, P. auriculata and P. zeylanica were investigated followed by multivariate statistical analyses and their antioxidant activity. Also, two alkylated phenols i.e., 2,6-di-tert-butyl phenol and 2,4-di-tert-butyl phenol not reported earlier from this taxon were isolated from P. indica. This metabolic study resulted in the identification of 25 and quantification of 18 metabolites. Principal component analysis showed the clear distinction among the three species. The antioxidant activity in the extracts was tested by free radical scavenging method. The three Plumbago species revealed interesting antioxidant potential, in particular, P. indica, which was rich in naphthoquinones, coumarins, alkylated phenols, sterols, triterpenes, fatty acids showed lowest IC50 value. The results highlighted the role of P. indica in the management of oxidative stress especially when they are utilized in the formation of fermented food products.

Optimization of the Duration and Intensity of UV-A Radiation to Obtain the Highest Free Phenol Content and Antioxidant Activity in Sprouted Sorghum (Sorghum bicolor L. Moench).

Technologies such as UV-A radiation applied to sprouted sorghum can stimulate the synthesis or release of phenolic compounds. Since the optimal conditions for stimulating the formation of these compounds in sorghum sprouts are unknown, we used the response surface methodology to identify the optimal conditions of irradiation duration and intensity to obtain the highest free phenol content and antioxidant activity in sprouted sorghum. The results showed that, compared with nonirradiated sorghum sprouts, sprouts irradiated under the optimal duration of 11.7 h and the optimal intensity of 5.4 µW/cm2 had a significantly higher phenol content (26.3%) and antioxidant activity as measured by DPPH (28.3%) and TEAC (21.1%) assays. Our findings suggest that UV-A radiation can help develop sorghum sprouts with high biological potential that can be used to produce healthy foods for human consumption.

New insights into the effect of fermentation temperature and duration on catechins conversion and formation of tea pigments and theasinensins in black tea.

BACKGROUND: The phenol oxidative pathway during fermentation remains unclear. To elucidate the effect of fermentation on phenol conversion, we investigated the effects of fermentation temperature and duration on the conversion of catechins and the formation of theasinensins (TSs), theaflavins (TFs), thearubigins (TRs), and theabrownins (TBs). RESULTS: During fermentation, TSs formation increased initially and then decreased. Long fermentation durations were unfavorable for liquor brightness (LB) and resulted in the production of large amounts of TRs and TBs. Low fermentation temperatures (20 °C and 25 °C) favored the maintenance of polyphenol oxidase activity and the continuous formation of TFs, TSs, and TRSI (a TRs fraction), resulting in better LB and liquor color. Higher temperatures (30 °C, 35 °C, and 40 °C) resulted in higher peroxidase activity, higher oxidative depletion rates of catechins, and excessive production of TRSII (a TRs fraction) and TBs. Analysis of the conversion pathway of polyphenolic compounds during fermentation showed that, during early fermentation, large amounts of catechins were oxidized and converted to TFs and theasinensin B. As fermentation progressed, considerable amounts of theaflavin-3'-gallate, theasinensin A, theaflavin-3-gallate, theaflavin-3,3'-digallate, and theasinensin C were produced and then converted to TRSI; in the final stage, TRSII and TBs were converted continuously. CONCLUSION: Different fermentation temperature and duration combinations directly affected the type and composition of phenolic compounds. The key conditions for controlling phenolic compound conversion and fermentation direction were 60 or 90 min and 25 or 30 °C. Our study provides insights into the regulation of phenolic compound conversion during black tea fermentation. © 2021 Society of Chemical Industry.

The signaling role of extracellular ATP in co-culture of Shiraia sp. S9 and Pseudomonas fulva SB1 for enhancing hypocrellin A production.

BACKGROUND: Adenosine 5'-triphosphate (ATP) plays both a central role as an intracellular energy source, and a crucial extracellular signaling role in diverse physiological processes of animals and plants. However, there are less reports concerning the signaling role of microbial extracellular ATP (eATP). Hypocrellins are effective anticancer photodynamic therapy (PDT) agents from bambusicolous Shiraia fungi. The co-culture of Shiraia sp. S9 and a bacterium Pseudomonas fulva SB1 isolated from Shiraia fruiting bodies was established for enhanced hypocrellin A (HA) production. The signaling roles of eATP to mediate hypocrellin biosynthesis were investigated in the co-culture. RESULTS: The co-culture induced release of eATP at 378 nM to the medium around 4 h. The eATP release was interdependent on cytosolic Ca2+ concentration and reactive oxygen species (ROS) production, respectively. The eATP production could be suppressed by the Ca2+ chelator EGTA or abolished by the channel blocker La3+, ROS scavenger vitamin C and NADPH oxidase inhibitor diphenyleneiodonium chloride (DPI). The bacterium-induced H2O2 production was strongly inhibited by reactive blue (RB), a specific inhibitor of membrane purinoceptors, but dependent on the induced Ca2+ influx in the co-culture. On the other hand, the application of exogenous ATP (exATP) at 10-300 µM to Shiraia cultures also promoted fungal conidiation and HA production, both of which were blocked effectively by the purinoceptor inhibitors pyridoxalphosphate-6-azophenyl-2', 4'-disulfonic acid (PPADS) and RB, and ATP hydrolase apyrase. Both the induced expression of HA biosynthetic genes and HA accumulation were inhibited significantly under the blocking of the eATP or Ca2+ signaling, and the scavenge of ROS in the co-culture. CONCLUSIONS: Our results indicate that eATP release is an early event during the intimate bacterial-fungal interaction and eATP plays a signaling role in the bacterial elicitation on fungal metabolites. Ca2+ and ROS are closely linked for activation of the induced ATP release and its signal transduction. This is the first report on eATP production in the fungal-bacterial co-culture and its involvement in the induced biosynthesis of fungal metabolites.

Storage Stability of Antioxidant in Milk Products Fermented with Selected Kefir Grain Microflora.

The aim of the study was to assess the antioxidant potential of goat's milk and whey from goat's milk fermented with selected bacteria strains from kefir grain (L. plantarum, L. fermentum, L. rhamnosus and L. acidophilus) with regard to fermented cow's milk with the same bacteria strains. The assessment of antioxidant potential was made by ABTS, DPPH, TPC and FRAP methods. The work also assessed metabolic activity of tested lactic acid bacteria using measurement of electrical impedance changes in the growing medium. The highest values describing the antioxidant potential were found for fermented milk by L. acidophilus. It was also found that the time of cooling storage causes significantly increasing the antioxidant potential of most analyzed samples. Metabolic activity of tested lactic acid bacteria was the highest for cow's milk. The course of curves for goat's milk and whey from goat's milk was similar, which confirms the differences between cow and goat milk.

The Potential of Virgin Olive Oil from cv. Chondrolia Chalkidikis and Chalkidiki (Greece) to Bear Health Claims according to the European Legislation.

The European food legislation authorizes the use of certain health claims based on a scientific basis. This study aimed to evaluate the fatty acid, tocopherol, and polar phenol composition of virgin olive oil (VOO) from cv. Chondrolia Chalkidikis and Chalkidiki regarding the fulfillment of official requirements for the health claims of 'oleic acid', 'vitamin E', and 'olive oil polyphenols'. The examination of representative industrial VOOs from 15 olive mills of the Chalkidiki regional unit showed that the two cultivars yield oils contained the necessary concentrations of the responsible bioactive compounds. This evidence was further substantiated by a four harvest study whereby olives from different maturity stages were sampled from three olive groves. Oils were extracted at a laboratory scale and examined for their content in the above-mentioned three categories of constituents. Oils produced at industrial scale from olives harvested on the 'technological optimum' stage according to the olive grove proprietor were also analyzed. Extra virgin olive oil of the studied cultivars can safely bear the generic claims for 'oleic acid' and 'vitamin E'. The cultivars present great potential regarding the total hydroxytyrosol and tyrosol content of the extracted oil required to attain the third health claim that may be influenced negatively by manufacturing practices.

Amino-based magneto-polymeric-modified mixed iron hydroxides for magnetic solid phase extraction of phenol residues in environmental samples.

Mixed iron hydroxides (MIHs) modified with different amino-based polymeric materials, including aminopropyltriethoxysilane, polydopamine, diaminobenzoic acid, polyaniline, and polyphenylenediamine, were comparatively investigated as sorbents for the extraction of phenol compounds. Polyphenylenediamine-modified mixed iron hydroxides (MIH@PPDA) showed high adsorption capability for most target analytes. Its ferromagnetic behavior, with a magnetization of 17.38 emu g-1, was sufficient for subsequent use in magnetic solid-phase extraction (MSPE). The functional groups, morphology, and magnetic properties of this magnetic nanomaterial were investigated using Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometry, X-ray diffraction, and CHN analysis. High-performance liquid chromatography with a photodiode array detector was used to quantify phenol compounds. The experimental parameters affecting the efficiency of the entire MSPE process were optimized. Good linearity in the range of 0.5-1000 µg L-1 was obtained (depended on the compound). The detection and quantitation limits varied from 0.01 to 0.3 µg L-1 and 0.03 to 0.9 µg L-1, respectively. The enrichment factors for all phenol compounds were in the range of 80-285. The precision in terms of intra- and inter-day relative standard deviations were below 5.8% and 6.2%, respectively. The developed MSPE method was applied to analyze phenol compounds in diverse samples, including soil, drinking water, and fruit. Relative recoveries of 76.7-130.1% were obtained. The MIH@PPDA magneto-polymeric sorbent exhibits good stability and is reliable for a variety of phenol compounds.

Validation of a phenol-sulfuric acid method in a microplate format for the quantification of soluble sugars in ruminant feeds.

Soluble sugars in feeds are important for ruminant production; however, performing numerous sugar analyses within a short period is a laborious task. Here, we developed a phenol-sulfuric acid (PSA) assay in a microplate format to quantify soluble sugars in ruminant feeds. This method is easy and quick and requires only a small quantity of harmful reagents. We found that assay measurements were not affected by the representative organic acids and sugar alcohol contained in feeds. The treatment of activated charcoal with ethanol extract prior to the PSA assay was effective in removing interfering compounds for a more accurate determination of soluble sugars in certain feeds. Furthermore, the inter-day and intra-day repeatability of the present method was acceptable. Hence, we conclude that the method developed in this study is suitable for routine analysis of soluble sugars content in ruminant feeds.

Antidiabetic profiling, cytotoxicity and acute toxicity evaluation of aerial parts of Phragmites karka (Retz.).

ETHNOPHARMACOLOGICAL RELEVANCE: Phragmites karka (Retz.) of family Poaceae is a pristine tropical plant that is well known to the local healers for ailments of diabetes, fever, diarrhea and CNS depression but lacks the scientific evidence behind its traditional usage. Hence, we explicated this plant to find the scientific basis of its traditional utilization. AIM OF THE STUDY: The current study aims to find out the antidiabetic potential, toxicity after oral administration and in vitro cytotoxic activity of aerial parts of the plant on HeLa cells. METHODS: The plant was extracted with methanol by maceration and the crude extract was then subjected to solvent partitioning with modified Kupchan method for preparing several fractions. Phytochemical screening and total phenolic content of the plant was first determined through established procedures. Acute toxicity of the plant was studied by orally administering a single high dose (5000 mg/kg) of drug. Cytotoxicity of the methanolic plant extract was determined by measuring the percentage of cell viability on human cervical cancer cell lines, HeLa. In vitro antidiabetic activity was determined through iodine starch and DNSA (3,5-dinitrosalicylic acid) method of α-amylase inhibition. Finally, in vivo oral glucose tolerance test and alloxan induced antidiabetic activity test was performed at 150 and 300 mg/kg body weight doses of plant extract to confirm the in vivo antidiabetic activity. RESULTS: No mortality was demonstrated by Phragmites karka in the acute toxicity test. However, signs of cellular toxicity was observed and histopathological studies on major organs exhibited necrosis in liver and kidney. In vitro cytotoxicity assay revealed the death of HeLa cells by DCM (dichloromethane) and n-hexane fractions of plant extract at 100 and 10 µg/mL concentrations. The IC50 value of the fractions were later evaluated by MTT assay (316.1 and 96.7 µg/mL for n-hexane and DCM fractions, respectively). In the iodine starch and DNSA method of α-amylase enzyme inhibitory activity test, substantial inhibition of enzyme was observed with the IC50 values of 2.05 and 2.08 mg/mL, respectively. In the in vivo antidiabetic activity test, considerable reduction in blood glucose level of diabetic mice was detected in both oral glucose tolerance test and alloxan induced antidiabetic activity test. In addition, the microscopic examination of pancreas showed noticeable recovery of pancreatic ß cells and the blood lipid profile analysis represented a significant (p < 0.05) reduction of total cholesterol, LDL (low density lipoprotein) and triglyceride level in plant extract treated mice. CONCLUSION: Results of this study reveals that the Phragmites karka extract is toxic at cellular level after oral administration and cytotoxic when tested on HeLa cells. The plant also evidenced hypoglycemic property, possibly through the inhibition of α-amylase enzyme and recovered the pancreatic beta cells along with the improvement of lipid profile of diabetic mice. However, robust studies on this plant is required to isolate the bioactive compounds, elucidate structures and evaluate their mechanism of actions in support of our findings. CLASSIFICATION: Toxicology and Safety, Quality Traditional Medicine.

Adsorption mechanism and effectiveness of phenol and tannic acid removal by biochar produced from oil palm frond using steam pyrolysis.

In order to meet the growing demand for adsorbents to treat wastewater effectively, there has been increased interest in using sustainable biomass feedstocks. In this present study, the dermal tissue of oil palm frond was pyrolyzed with superheated steam at 500 °C to produce nanoporous biochar as bioadsorbent. The effect of operating conditions was investigated to understand the adsorption mechanism and to enhance the adsorption of phenol and tannic acid. The biochar had a microporous structure with a Brunauer-Emmett-Teller surface area of 422 m2/g containing low polar groups. The adsorption capacity of 62.89 mg/g for phenol and 67.41 mg/g for tannic acid were obtained using 3 g/L biochar dosage after 8 h of treatment at solution pH of 6.5 and temperature of 45 °C. The Freundlich model had the best fit to the isotherm data of phenol (R2 of 0.9863), while the Langmuir model best elucidated the isotherm data of tannic acid (R2 of 0.9632). These indicated that the biochar-phenol interface was associated with a heterogeneous multilayer sorption mechanism, while the biochar-tannic acid interface had a nonspecific monolayer sorption mechanism. The residual concentration of 26.3 mg/L phenol and 23.1 mg/L tannic acid was achieved when treated from 260 mg/L three times consecutively with 1 g/L biochar dosage, compared to a reduction to 72.3 mg/L phenol and 69.9 mg/L tannic acid using 3 g/L biochar dosage in a single treatment. The biochar exhibited effective adsorption of phenol and tannic acid, making it possible to treat effluents that contain varieties of phenolic compounds.

Exhaled breath analysis using on-line preconcentration mass spectrometry for gastric cancer diagnosis.

Breath volatile biomarkers are capable of distinguishing patients with various cancers. However, high throughput analytical technology is a prerequisite to a large-cohort study intended to discover reliable breath biomarkers for cancer diagnosis. Single-photon ionization (SPI) is a universal ionization technology, and SPI-mass spectrometry (SPI-MS) shows a remarkable advantage in the comprehensive detection of volatile organic compounds (VOCs), in particular, nonpolar compounds. In this study, we have introduced SPI-MS coupled with on-line thermal desorption (TD-SPI-MS) to demonstrate nontarget analysis of breath VOCs for gastric cancer patients. The breath fingerprints of the gastric cancer patients were significantly distinct from that of the control group. Acetone, isoprene, 1,3-dioxolan-2-one, phenol, meta-xylene, 1,2,3-trimethylbenzene, and phenyl acetate showed higher relative peak intensities in the breath profiles of gastric cancer patients. A diagnostic prediction model was further developed by using a training set (121 samples) and validated with a test set (53 samples). The predication accuracy of the developed model was 96.2%, and the area under the curve (AUC) of the receiver operator characteristic curve (ROC) was 0.997, indicating a satisfactory prediction ability of the developed model. Thus, by taking gastric cancer as an example, we have shown that TD-SPI-MS will be a promising tool for high throughput analysis of breath samples to discover characteristic VOCs in patients with various cancers.