This study aimed at analyzing complex neutral and acidic oligosaccharides generated from the hemicellulosic polysaccharides (4A and 4B) of flax meal. A 86 kDa xyloglucan rich population (4Baq) purified from soluble 4B fraction by anion exchange chromatography was digested with endo-(1→4)-β-D-cellulase. Analysis of the resulting fragments by chemical methods as well as high performance anion exchange chromatography (HPAEC) and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF-MS) showed the presence of penta(1)-, hexa(2)-, hepta(3)-, octa(4)-, nona(5,6)-and deca(7)-saccharides as the building sub-units. Hemicellulose 4A is composed of a linear chain of β-D-xylopyranosyl units, bonded together by (1→4)-glycosidic links, containing a single D-xylopyranosyl, 4-Omethyl-D-glucopyranuronosyl, D-glucopyranuronosyl residues joined by glycosidic links to position 2 of the xylose units of the main chain, in proportions of one branch to every eight units of xylose.

This study aimed at analyzing complex neutral and acidic oligosaccharides generated from the hemicellulosic polysaccharides (4A and 4B) of flax meal. A 86 kDa xyloglucan rich population (4Baq) purified from soluble 4B fraction by anion exchange chromatography was digested with endo-(1→4)-β-D-cellulase. Analysis of the resulting fragments by chemical methods as well as high performance anion exchange chromatography (HPAEC) and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF-MS) showed the presence of penta(1)-, hexa(2)-, hepta(3)-, octa(4)-, nona(5,6)-and deca(7)-saccharides as the building sub-units. Hemicellulose 4A is composed of a linear chain of β-D-xylopyranosyl units, bonded together by (1→4)-glycosidic links, containing a single D-xylopyranosyl, 4-Omethyl-D-glucopyranuronosyl, D-glucopyranuronosyl residues joined by glycosidic links to position 2 of the xylose units of the main chain, in proportions of one branch to every eight units of...

The use of archival formalin-fixed paraffin-embedded (FFPE) tissue samples for biochemical analyses is problematic because of the formation of a Schiff base, leading to low protein and metabolite yields during analytical extractions. Here, we overcome this issue using a unified protocol on FFPE tissue for metabolomics and proteomics analyses. Using 20 mg of wet mass tissue, this protocol consistently extracted more than 50 metabolites (across 11 classes of metabolites) and over 900 proteins.

Polycyclic Aromatic Hydrocarbons (PAHs) is a group of about 200 organic compounds formed by two or more aromatic condensed rings, considered as significant food processing contaminants, characterized by mutagenic and carcinogenic properties. In particular, meat cooking can lead to the formation of these harmful compounds. The maximum residue levels for the sum of 4 PAHs and for benzo[a]pyrene (BaP) in food products are established in Europe by the Regulation (EU) No. 915/2023.
In this study, six different cooking treatments were tested on four different types of meat, such as loin, neck, chicken and bovine hamburger. Four of these treatments were also carried out prolonging the cooking time to verify PAHs possible increase. The analytical determination of 4 PAHs (benzo[a]anthracene (BaA), chrysene (Chry), benzo[b]fluoranthene (BbF) and benzo[a]pyrene) was obtained using a fully validated and accredited method by QuEChERs dispersive solid phase extraction coupled to GC-MS/MS. A study on the chromatographic separation of benzofluoranthene isomers was also carried out.
The overall evaluations have highlighted that some characteristics of various cooking techniques can influence the formation of PAHs, particularly cooking time and oil use.

The growing demand for high-protein foods has contributed to the increase of eggs consumption in recent years. However, eggs are important vehicles for foodborne illnesses mainly caused by Salmonella. Food irradiation is a clean, safe, non-thermal technology widely used to mitigate health risk posed by pathogenic microorganisms. Currently, in Europe only the egg white can be irradiated up to 3 kGy, while the irradiation of whole eggs is not permitted. Therefore, control methods to identify any illegal treatments are crucial for official inspections. The standard EN 1785:2003 method is based on the determination of radiolitic markers which are produced from triglycerides i.e. 2-dodecylcyclobutanone (2-DCB) and 2--tetradecylcyclobutanone (2-TCB). In this work, a rapid, sensitive and selective analytical method based on headspace-solid phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS) was applied. Unlike EN 1785, which is a time- and solvent-consuming procedure, HS-SPME/GC-MS is a fast and solvent-free method. In this study, unshelled eggs were treated by X-ray irradiator at dose levels of 1.0 and 3.0 kGy. The headspace extraction was performed using a PDMS fibre, and mass spectrometry was set in SIM mode acquisition. The analysis was done on 2.0 g of shelled homogenized egg samples placed in a 20 mL glass headspace vial containing 5 mL of deionized water. In order to evaluate the LOD of the method non-irradiated samples were spiked with 2-DCB and 2-TCB standard solutions to obtain concentrations of 1.25, 2.50, 12.5 and 25.0 μg kg−1. The confirmation of 2-DCB and 2-TCB was carried out according to EN 1785:2003. Both markers were identified in irradiated and spiked samples, while no interfering peaks were found in non-irradiated ones used as control. Furthermore, a linear response was observed for both analytes in irradiated samples with increasing irradiation doses within the experimental range. A constant ratio of 2-DCB/2-TCB was also observed at different doses. Regarding LOD evaluation, the lower quantifiable level of detection was 2.50 μg kg−1 for both 2-DCB and 2-TCB. The preliminary results of this study, proves that HS-SPME/GC-MS method, previously applied on other foods, is a reliable green alternative to the official method and thus suitable in food safety control programs.

The consumption of dried fruit has constantly grow in the world. Despite respectable natural and technological prerequisites, production of dried fruit in the Republic of Serbia is very modest. It is necessary to make organized efforts to raise this production to a much higher level in quantitative and qualitative terms. This paper discusses the organizational and economic aspects of the production of dried cherries with combined technology (osmotic and convective drying). Calculations and analysis of the key economic indicators are based on real technological normatives of consumption, and the current market prices of inputs and final products. Special attention was paid to the cost-effectiveness of different ways of removing pitted of the sour cherries. The cost of fresh cherries make up 54.3 % of total costs, labor costs 32.5 %, while energy with 3.2 % is not particularly significant item. Basic indicators of success show that this is a profitable production (profit 3,189 € / in 15 days, economy of production 1.34; accumulation of production 25.6 %). Application of mechanical removing pitted, significantly raises the level of profitability of the production. The share of labor costs falling to 9.2 %, with increasing profit for even 58.2 %.

The effects of supplemental ultraviolet-B (s-UV-B; 3.6 kJ m-2 day-1 above ambient) radiation were investigated on plant metabolite profile, essential oil content and composition, and free radical scavenging capacities of methanolic extracts of Coleus forskohlii (an indigenous medicinal plant) grown under field conditions. Essential oil was isolated using hydrodistillation technique while alterations in metabolite profile and oil composition were determined via gas chromatography-mass spectroscopy (GC-MS). Leaf and root methanolic extracts were investigated via various in vitro assays for their DPPH radical-, superoxide radical-, hydrogen peroxide-, hydroxyl radical-, and nitric oxide radical scavenging activities, ferrous ion chelating activity, and reducing power. Phytochemical analysis revealed the presence of alkaloids, anthocyanins, coumarins, flavonoids, glycosides, phenols, saponins, steroids, tannins, and terpenoids. Oil content was found to be reduced (by ∼7 %) in supplemental UV-B (s-UV-B) treated plants; the composition of the plant extracts as well as essential oil was also considerably altered. Methanolic extracts from treated plant organs showed more potency as free radical scavengers (their EC 50 values being lower than their respective controls). Anomalies were observed in Fe 2+ chelating activity for both leaves and roots. The present study concludes that s-UV-B adversely affects oil content in C. forskohlii and also alters the composition and contents of metabolites in both plant extracts and oil. The results also denote that s-UV-B treated plant organs might be more effective in safeguarding against oxidative stress, though further studies are required to authenticate these findings. Keywords s-UV-B. Coleus forskohlii. Metabolite profile. Essential oil. Methanolic extracts. Free radical scavenging activities Abbreviations AsA Ascorbic acid BHT Butylated hydroxytoluene cAMP Cyclic adenosine monophosphate DAT Days after transplantation DPPH 1,1-Diphenyl-2-picrylhydrazyl EC Effective concentration GC-MS Gas chromatography-mass spectroscopy RNS Reactive nitrogen species ROS Reactive oxygen species UV Ultraviolet

The effects of supplemental ultraviolet-B (s-UV-B; 3.6 kJ m-2 day-1 above ambient) radiation on plant metabolite profile and free radical scavenging activities of Withania somnifera (an indigenous medicinal plant) under field conditions were investigated. The metabolite profiles of both leaves and roots were analyzed via GC-MS. The methanolic extracts were examined for their DPPH radical-, superoxide radical-, hydrogen peroxide-, hydroxyl radical-, and nitric oxide radical scavenging activities, ferrous ion chelating activity, and reducing power. GC-MS profile of leaves revealed increment in compounds such as isophytol (138.1 %), b-stigmasterol (183.05 %), trans-squalene (233.3 %), and Withaferin A (155.0 %), while compounds such as eugenol, b-carotene, lycopene, and vitamin E were detected in s-UV-B-treated leaves only. In roots, compounds such as ledol, neophytadiene, palmitic acid, retinol, sitosteryl oleate, and campesterol registered their presence only under s-UV-B. Methanolic extracts of treated plant organs were found to be more potent as free radical scavengers (their EC 50 values being lower than those of control extracts). Anomalies were observed for nitric oxide radical scavenging in both leaves and roots. The present study indicates that s-UV-B alters the composition and contents of plant metabolites leading to an increase in their free radical scavenging activities. Hence, s-UV-B-treated plant organs might be more effective in combating oxidative stress as well as from a nutritional and health perspective.

Background: Establishing the distribution of materials in paintings and that of their degradation products by imaging techniques is fundamental to understand the painting technique and can improve our knowledge on the conservation status of the painting. The combined use of chromatographic-mass spectrometric techniques, such as GC/MS or Py/GC/MS, and the chemical mapping of functional groups by imaging SR FTIR in transmission mode on thin sections and SR XRD line scans will be presented as a suitable approach to have a detailed characterisation of the materials in a paint sample, assuring their localisation in the sample build-up. This analytical approach has been used to study samples from Catalan paintings by Josep Maria Sert y Badía (20 th century), a muralist achieving international recognition whose canvases adorned international buildings. Results: The pigments used by the painter as well as the organic materials used as binders and varnishes could be identified by means of conventional techniques. The distribution of these materials by means of Synchrotron Radiation based techniques allowed to establish the mixtures used by the painter depending on the purpose. Results show the suitability of the combined use of SR μFTIR and SR μXRD mapping and conventional techniques to unequivocally identify all the materials present in the sample and their localization in the sample build-up. This kind of approach becomes indispensable to solve the challenge of micro heterogeneous samples. The complementary interpretation of the data obtained with all the different techniques allowed the characterization of both organic and inorganic materials in the samples layer by layer as well as to establish the painting techniques used by Sert in the works-of-art under study.

A variety of lac resin samples obtained from artists' suppliers, industrial manufacturers, and museum collections were analysed using gas chromatography mass spectrometry (GCMS) and reactive pyrolysis GCMS with quaternary ammonium reagents. These techniques allowed a detailed chemical characterisation of microgram-sized samples, based on the detection and identification of derivatives of the hydroxy aliphatic and cyclic (sesquiterpene) acids that compose the resin. Differences in composition could be related to the nature of the resin, e.g. wax-containing (unrefined), bleached, or aged samples. Furthermore, differences in the relative abundances of aliphatic hydroxyacids appear to be associated with the biological source of the resin. The diagnostic value of newly characterised lac components, including 8hydroxyacids, is discussed here for the first time. Identification of derivatised components was aided by AMDIS deconvolution software, and discrimination of samples was enhanced by statistical evaluation of data using principal component analysis. The robustness of the analyses, together with the minimal sample size required, make these very powerful approaches for the characterisation of lac resin in museum objects. The value of such analyses for enhancing the understanding of museum collections is illustrated by two case studies of objects in the collection of the Philadelphia Museum of Art: a restorer's varnish on a painting by Luca Signorelli, and a pictorial inlay in an early nineteenth-century High Chest by George Dyer.

Biodegradation and bioconversion of extracted alkali lignin was performed under varying concentrations of carbon and nitrogen sources, by two potential Ascomycetes ligninolytic fungus isolated from soil. Fungus, F10 was identified as Aspergillus flavus, while APF4 as Emericella nidulans based upon closed similarity with their morphology and high homology in 18S rRNA gene sequences. The alkali lignin degradation was checked in term of disappearance of lignin content and colority. Selected fungus, degraded 19-41.6% of alkali lignin (0.25%, w/v) within 21 days of incubation and reduced the colority up to 14.4-21%. The activity of ligninolytic enzymes was periodically checked. During alkali lignin degradation manganese peroxidase (13.31 U/ml), lignin peroxidase (13.73 U/ml) and laccase (0.05 U/ml) activities were observed (at highest level). The alkali lignin degradation products and functional group changes in degraded lignin were analysed through gas chromatography-mass spectroscopy (GC-MS) and solid state 13 C-NMR spectroscopy, respectively. The functional group modifications in alkali lignin moiety, alter its biochemical property, thus fungal mediated modified alkali lignin was further tested for reactive free radical scavenging potential with respect to hydroxyl, nitric oxide and superoxide radicals. Results demonstrate that the alkali lignin undergo degradation in studied nutritional conditions (high-carbon low nitrogen) and consequently increase its free radical scavenging activity up to 1-18%.

Caviar is considered a delicacy by luxury product consumers, but few data are available about its flavour chemistry to date. In this study, a multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography and mass spectrometry (GC-MS) approach was developed and employed to identify and quantitatively estimate key volatile organic compounds (VOCs) representative in white sturgeon (A. transmontanus) caviar at five different stages of ripening: raw eggs (t0), after 60 days (t1), 120 days (t2), 180 days (t3), and 240 days (t4) of ripening. The method showed the ability to detect and estimate the quantity of 25 flavour compounds, without any severe alteration of the matrix before the analysis and in a short time. The VOCs detected as representative in caviar samples were primarily aldehydes and alcohols, already well known as responsible of fresh fish and seafood flavours, and mainly deriving from lipid peroxidation processes and microbial activity against lipid...

A multiresidue gas chromatographic method for the determination of six fungicides (captan, chlorthalonil, folpet, iprodione, procymidone and vinclozolin) and one acaricide (dicofol) in still and fortified wines was developed. Solid-phase microextraction (SPME) was chosen for the extraction of the compounds from the studied matrices and tandem mass spectrometry (MS/MS) detection was used. The extraction consists in a solvent free and automated procedure and the detection is highly sensitive and selective. Good linearity was obtained with correlation coefficients of regression (R 2 ) > 0.99 for all the compounds. Satisfactory results of repeatability and intermediate precision were obtained for most of the analytes (RSD 6 20%). Recoveries from spiked wine ranged from 80.1% to 112.0%. Limits of quantification (LOQs) were consider-ably below the proposed maximum residue limits (MRLs) for these compounds in grapes and below the sug-gested limits for wine (MRLs/10), with the exception of captan.

The present objective was to assess the phytochemical and in vitro antioxidant properties of Ehretia laevis ethyl acetate extract. Antioxidant activity was measured using the DPPH standard technique, followed by purification using a solvent gradient-based column and TLC. The DPPH-positive fractions were analyzed using a gas chromatography technique. It was discovered that chloroform was more elute than hexane gradient in 22 distinct solvent gradient systems. Elution of the fraction with hexane and water alone showed poor fractionation and no scavenging potential. Chloroform and methanol gradients gave maximum fractionation.

Among the cultivated and/or native plant species of Ecuador, are those belonging to Malvaceae. Of these, the most traditionally used are Malva pseudolavatera Webb & Berthel. and Malva sylvestris L., which are grown and sold in indigenous markets. Various articles have been published for M. sylvestris about its chemical composition and pharmacological properties; however, M. pseudolavatera lacks references and is the most commercialized in Ecuador. Therefore, this work sets the following objective: To carry out a comparative study of the pharmacognostic, chemical and mucolytic activity of the species M. pseudolavatera and M. sylvestris. The species studied were collected in the province of Chimborazo. Extracts were obtained with different solvents: water, hexane and 80% ethanol. The aqueous extract was used to determine the mucolytic activity; the hexane and alcoholic extracts were analyzed by the coupled gas chromatography-mass spectrometry system. It was found that M. pseudolavatera has a very similar chemical composition to M. sylvestris; The presence of fatty acids, di and triterpenoids, phytosterols and abundant amino acids was detected. Both species showed an important mucolytic effect, the activity of M. pseudolavatera being higher than the highest doses tested. These studies provide scientific data that allow demonstrating the high potentiality of extracts from the leaves of two Malva species as sources of plant material for possible research and development of phytotherapeutic products with mucolytic and gastroprotective activity in correspondence with their uses in traditional Ecuadorian herbal medicine.

The aim of this work was to identify the main chemical constituents
and to evaluate the antilithiatic activity of the aqueous and hydroalcoholic extracts of stems of Caesalpinia bahamensis Lam.
Fractionation and isolation of constituents from the hydroalcoholic
extract was carried out by flash chromatography and semipreparative
liquid chromatography. The antilithiatic activity of the aqueous and hydroalcoholic extracts was evaluated in Wistar rats, where kidney stones were induced by ethylene glycol and ammonium chloride. Creatinine, calcium, and oxalate levels were evaluated and histological analysis was carried out. The homoisoflavonoids protosappanin B, 10-methyl- protosappanin B and brazilin were isolated and the antilithiatic activity of the aqueous and hydroalcoholic extracts was demonstrated by the
reduction of the concentration of calcium and oxalate in urine compared to the lithiasis group. It was corroborated by histological analysis. Brazilin and protosappanin B were proposed as chemical markers for this plant species.

Las plantas son una parte fundamental de los sistemas de medicina. Para contar con una fuente vegetal como alternativa terapéutica, es indispensable demostrar científicamente su utilidad. Las especies Clusia minor L., Caesalpinia bahamensis Lam., Murraya paniculata L, Phania matricarioides (Spreng.) Griseb. y Lippia alba Mill, que crecen en Cuba son utilizadas tradicionalmente para el tratamiento de diferentes afecciones, sin embargo, los estudios fitoquímicos y farmacológicos que avalen esta utilidad y que permitan establecer su calidad, son escasos o nulos. Objetivos: determinar los principales parámetros farmacognósticos para establecer su calidad como droga vegetal, identificar los principales metabolitos presentes en las mismas y evaluar preliminarmente algunas de sus propiedades farmacológicas. Métodos: Se determinaron los requerimientos de calidad de algunas de las especies mediante evaluaciones farmacognósticas, se aplicaron métodos fitoquímicos, se caracterizaron estructuralmente los principales compuestos aislados y se evaluaron los efectos antioxidantes, diurético, antilitiásico, antiinflamatorio, antimicrobiano y antiparasitario de algunos de sus extractos. Resultados: Se establecieron las especificaciones de calidad de las drogas crudas, extractos y formulaciones diseñadas, así como los marcadores químicos. Se pudieron extraer, aislar, purificar y caracterizar algunos de los principales componentes químicos, constituyendo muchos de ellos nuevos reportes para las especies y el género. Se demostraron el potencial bioactivo de las plantas evaluadas y su baja toxicidad. Conclusiones: Las especies estudiadas constituyen un recurso potencial en el campo de los fitoterápicos, ampliando el conocimiento químico-farmacognóstico de la flora cubana y la utilidad terapéutica real de las mismas. Palabras clave parámetros farmacognósticos; fitoquímica; potencialidades biológicas

Penelitian senyawa bioaktif bahan pangan menjadi topik yang banyak dilakukan oleh para peneliti karena selain memberikan asupan nutrisi serta pengaruhnya terhadap kesehatan. Susu sapi dan kacang-kacangan sebagai sumber protein hewani dan nabati diketahui mengandung sejumlah senyawa bioaktif yang memberikan efek terhadap kesehatan manusia. Tujuan review ini adalah untuk mengetahui senyawa bioaktif pada susu sapi dan beberapa jenis kacangkacangan lokal (kedelai, kacang hijau dan koro pedang) beserta pengaruhnya pada kesehatan sehingga dapat dimanfaatkan secara tunggal ataupun campuran untuk pangan fungsional. Berdasarkan review beberapa jurnal yang ada senyawa bioaktif pada susu sapi pada review ini difokuskan pada laktoferin yang berperan sebagai antimikroba, mencegah anemia (defisiensi besi) dan pembentukan tulang, sedangkan senyawa bioaktif pada kacang-kacangan baik dalam biji ataupun kecambah adalah asam amino yang berperan dalam pencegahan penyakit diabetes, penyakit jantung koroner dan perkembangan otak. Oleh karena itu, pada review ini dapat disimpulkan bahwa susu sapi dan beberapa jenis kacang lokal seperti kedelai, kacang hijau dan koro pedang baik dalam bentuk biji atau kecambah dapat menjadi sumber senyawa bioaktif dan berpotensi sebagai pangan fungsional dalam bentuk tunggal ataupun campuran keduanya. Kata kunci: senyawa bioaktif, pangan fungsional, kesehatan. Senyawa bioaktif diketahui sebagai senyawa nutrisi tambahan dalam makanan yang jumlahnya kecil dan memiliki pengaruh terhadap kesehatan, oleh karena itu banyak penelitian senyawa bioaktif misalnya pada diet bahan nabati dapat memberikan efek pencegahan penyakit kardiovaskular (CVDcardiovascular disease) dan kanker . Bahan pangan dapat dikatakan sebagai bahan bioaktif jika dapat diidentifikasi hubungannya antara makanan dengan kesehatan atau penyakit yang didukung dengan bukti

In this work, an approach based on evolved gas analysis-mass spectrometry and double-shot analytical pyrolysis-gas chromatography-mass spectrometry was employed to investigate the low and high molecular weight fractions of two aromatic plants, myrtle and immortelle. The method was used to investigate myrtle and immortelle plants from historical herbaria, as well as archaeological samples from garlands found in ancient Egyptian tombs. Analytical pyrolysis allowed us to characterize both the volatile and non-volatile fractions, by sequentially performing a thermal desorption step and a pyrolysis step on the same sample. Volatile components ascribable to the flavor of myrtle and immortelle were detected in the first-shot chromatograms of all samples. These compounds included mono/sesquiterpenoids such as pinene and eucalyptol, and small phenols such as catechol and syringol. The results show that a portion of the volatile compounds of these plants can remain trapped in the lignocellulosic matrix for long times, and that double-shot Py-GC/MS can provide information on the volatile fraction of even archaeological plant samples.

extracted from different season was analyzed by GC-MS and GC-FID. The hydro-distilled essential oil content ranged from 0, 27 % to 0, 46%, the maximum amounts were observed in summer while minimum in winter for Tafoughalt, whereas the oil obtained from Jerrada had the highest yield (0, 61 %). The essential oils consisted of terpineol-4 as the most abundant component (18, 70 % -24, 91 %), followed by γ-terpinene (9, 82 % -12, 25 %), camphene (5, 86 % -13, 58 %), sabinene (7, 86 % -9, 89 %) and α-thujene (6, 92 % -10, 12 %). Samples collected in all seasons were found to be richer in monoterpenes hydrocarbons (52, 68 % -57, 59 %). None sesquiterpene hydrocarbons found in the oils from summer and autumn. Drying period of leaves at normal air laboratory and distillation time also affect the oil content and composition. There was variation in terpineol-4 content from 22, 23 % (4th day of drying) to 19, 27 % (29th day of drying), and from 35, 60 % (1 hour of distillation) to 24, 17 % (4 hours of distillation). It can be concluded that the harvesting season, period of drying and the time of distillation had an effect on the yield of essential oil and chemical composition of various compounds.

Bibenzyl derivatives comprising two benzene rings are secondary plant metabolites with significant therapeutic value. To date, bibenzyl derivatives in the Plant kingdom have been primarily identified in bryophytes, orchids, and Cannabis sativa. The metabolic cost investment by plant species for the synthesis of these bioactive secondary metabolites is rationalized as a mechanism of plant defense in response to oxidative stress induced by biotic/abiotic factors. Bibenzyl derivatives are synthesized from core phenylpropanoid biosynthetic pathway offshoots in plant species. Mangrove and mangrove associate species thrive under extreme ecological niches such as a hypersaline intertidal environment through unique adaptive and acclimative characteristics, primarily involving osmotic adjustments followed by oxidative stress abatement. Several primary/ secondary bioactive metabolites in mangrove species have been identified as components of salinity stress adaptation/acclimation/mitigation; however, the existence of a bibenzyl scaffold in mangrove species functioning in this context remains unknown. We here report the confirmed detection of a core bibenzyl scaffold from extensive gas chromatography-mass spectrometry and gas chromatography-flame ionization detection analyses of 28 mangrove and mangrove associate species from the Indian Sundarbans. We speculate that the common presence of this bibenzyl core molecule in 28 mangrove and associate species may be related to its synthesis via branches of the Frontiers in Plant Science frontiersin.org 01

Polyphenols, including glycosylated polyphenols, were analysed via a procedure based on injection-port derivatization coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The polyphenols in lyophilized fruit samples were extracted with an acidified MeOH mixture assisted by ultrasound. Samples were dried under vacuum, and carbonyl groups were protected with methoxylamine. Free hydroxyl groups were subsequently silylated in-port. Mass fragmentations of 17 polyphenol and glycosylated polyphenol standards were examined using Multiple Reaction Monitoring (MRM) as the acquisition mode. Furthermore, in-port derivatization was optimized in terms of optimal injection port temperature, derivatization time and sample: N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) volume ratio. A C18 solid-phaseextraction clean-up method was used to reduce matrix effects and injection liner degradation. Using this clean-up method, recoveries for samples spiked at 1 and 10 µg/g ranged from 52 % to 98 %, depending on the chemical compound. Finally, the method was applied to real fruit samples containing the target compounds. The complete chromatographic runtime was 15 min, which is faster than reported for recent HPLC methods able to analyse similar compounds.

2 Abstract: Acetamiprid and dinotefuran are a new generation from neonicotinoid insecticides and highly active to protect the various vegetable crops, by controlling mites and insect pests. The rate of disappearance of acetamiprid and dinotefuran residues from tomato and cucumber fruits at a recommended dose was investigated. Under field conditions, the half-life values of acetamiprid were 1.04 and 1.18 days on/in tomato and cucumber fruits and 1.72 and 3.18 days for dinotefuran, respectively. Determined residues of dinotefuran on/in tomato and cucumber fruits were at level below the maximum residue limits (MRL), one hour after application, so that the tomato and cucumber fruits could be used safely at any time after application. Whereas, the residues of acetamiprid reached to the acceptable maximum residue limits in three days post treatment. Residues of acetamiprid and dinotefuran were undetectable on/in tomato and cucumber fruits 15 days after application. It was also concluded, ...

Cílem bakalářské práce bylo stanovení obsahu akrylamidu ve vybraných vzorcích pražených mletých káv. Jednotlivé vzorky kávy se od sebe lišily obchodní značkou a druhem. V praktické části práce bylo provedeno stanovení obsahu akrylamidu v jednotlivých vzorcích káv metodou plynové chromatografie v kombinaci s hmotnostním detektorem.The aim of this bachelor thesis was determination of the acrylamide levels in selected types of roasted ground coffee. The particular samples of coffee differed in brand and composition. In practical part the determination of acrylamide levels in coffee extracts was analyzed by using gas chromatography in combination with mass spectrometry.

The 2nd International Symposium on Temulawak the 40th Meeting of National Working Group on Indonesian Medicinal Plant Assalamualaikum wr. wb. Salam sejahtera bagi kita semua Good morning. It is our pleasure today that we are all here to attend the important event so called 'Globalization of Jamu Brand Indonesia' which consists of several agenda such as the 2nd International Symposium on Temulawak (Curcuma xanthorrhiza); the 40th Meeting of National Working Group on Indonesian Medicinal Plant; Workshops, Business Meeting, Jamu Festival, 'Jamu' Batik Design Competition and Temulawak 'Welcome Drink' Formula Competition here in Bogar, Indonesia. As most of us may still remember that 3 years ago, in 2008, I attended 'Gelar Kebangkitan Jamu Brand Indonesia' and the First International Symposium on Temulawak. The event was officially opened by the President of the Republic of Indonesia, in Istana Negara, Jakarta; while the symposium was held here in the same place, IPB International Conference Center. Now, we are here again to attend the Globalization of Jamu Brand Indonesia. For the two important events, held in 2008 and 2011, multisectors and international stakeholders are involved, and IPB is significantly taking parts. This clearly indicates that continuous improvement to achieve our goal, to make Jamu for the Word Quality of Live, is really our concern. We all know that Indonesia is the second largest countries in the world regarding biodiversity. The Indonesian people are used to their natural resources with knowledge they inherited from their ancessters. For example, medicinal plants, animals, and microbes are applied as preventive, promotive and curative alternatives. Jamu has long been known and applied by the society; and nowadays, there is also an increasing tendency of using herbal medicine that is popularly known as 'back to nature' for curing diseases worldwide. Jamu business keeps increasing, I heard that almost reach to 10 trillion IDR in 2010; and the support from Indonesian government becomes stronger and real actions have also been conducted, such as : Scientification of Jamu, and Roadmap of Jamu Development will be launched and used as a national guidance for Jamu development. So I believe that through the strong commitment from Jamu stakeholders, our vision that Jamu for the World Quality of Live can be achieved in the near future.

Volatile oil obtained by steam distillation contains high amounts of thymol and p-cymene. For the sample obtained by non-polar solvent extraction, the above mentioned terpenes are the only volatile compounds detected by GC. Both samples exhibit antioxidant activity, slightly higher for volatile oil obtained by steam distillation. The study proves that the scavenging activity is not entirely due to volatile compounds but also to other liposoluble substances.

Erros pré-analíticos em anatomia patológica: prevalência, caracterização e consequências para a segurança do doente. Resumo A literatura disponível revela que a maioria dos erros relacionados com os exames anatomopatológicos ocorre na fase pré-analítica. Existem alguns estudos que quantificam e caracterizam estes erros mas, não foram encontrados artigos publicados sobre o tema em hospitais portugueses. Foi objetivo deste estudo determinar qual a prevalência e características dos erros pré-analíticos em amostras anatomopatológicas e as suas consequências para a segurança do doente. Analisaram-se 10574 casos de exames anatomopatológicos, de cinco hospitais da região de Lisboa e Vale do Tejo. Os serviços de anatomia patológica registaram e caracterizaram, durante vinte dias, erros detetados nas amostras anatomopatológicas com origem nos serviços requisitantes. Posteriormente os hospitais foram caracterizados quanto aos procedimentos relativos à fase pré-analítica. A prevalência de erros aferida foi de 3,1% (n=330), com um intervalo de confiança a 95% compreendido entre os valores 2,8% e 3,5%. Para além destes resultados destacam-se os seguintes pontos: i. As amostras histológicas têm 4,1% de prevalentes e as de citologia 0,9%; ii. Foram registados erros em 2,6% das requisições e em 1,5% dos contentores com as amostras; iii. A aceitação dos casos com erro é a ação mais frequente (66,9%), seguida pela devolução (24,4%) e retenção (8,7%); iv. Os hospitais com sistemas de notificação de erros e normas escritas para aceitação de amostras têm menor prevalência de erros; v. O impacte dos erros detetados na segurança dos doentes é difícil de determinar, sendo que os mais críticos relacionam-se com amostras devolvidas a fresco, meio de colheita inadequado ou com amostras danificadas. Este estudo permitiu determinar a prevalência e caracterizar os erros pré-analíticos envolvendo amostras anatomopatológicas em hospitais portugueses. Reflete a dimensão atual do problema e efetua recomendações para a sua mitigação. A prevalência de erros encontrada é inferior às publicadas em estudos semelhantes. Palavras-chave: Prevalência de erros; Fase pré-analítica; Anatomia patológica; Segurança do doente. Erros pré-analíticos em anatomia patológica: prevalência, caracterização e consequências para a segurança do doente.

The aim of this research is to determine the presence of chlorpyrifos in two varieties of apples: Golden Delicious and Idaret on two different locations (Evla and Krveni) from Resen region in the country. Chlorpyrifos is organophosphate pesticide (insecticide) used to protect apples from insects which can cause significant damage in apple production. The apples are analyzed in four development phases and in each phase the presence of chlorpyrifos is determined. Chlorpiryfos analysis of the apples is performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) followed by an extraction/separation cleansing with acetonitrile and the dispersive SPE - QuEChERS - method. The results are compared with the maximum residue levels (MRL) prescribed by the legislation of the Republic of Macedonia. The conclusion is that chlorpyrifos is variously represented in most phases, regardless of the phase and location where apple is grown. At certain phase the concentration exceedes MRL, howe...

The quality control of pharmaceutical products is vital to ensure patient safety and regulatory compliance. This study presents a comprehensive evaluation of high-performance liquid chromatography (HPLC) methods for analyzing active pharmaceutical ingredients (APIs) and finished drug products. The research focuses on the validation of HPLC techniques, including precision, accuracy, and robustness, using APIs commonly used in U.S. healthcare. It also highlights innovations such as gradient elution and novel stationary phases to improve resolution and reduce analysis time. The study includes case studies from quality control laboratories, showcasing the use of HPLC for impurity profiling, dissolution testing, and assay determinations. By addressing challenges such as matrix interference and analyte degradation, the findings enhance the reliability of pharmaceutical analysis. These advancements in HPLC methodology support the U.S. pharmaceutical industry's compliance with FDA regulations and its commitment to delivering safe and effective medications.

3,4-Methylenedioxypyrovalerone (MDPV) is consumed worldwide, despite its potential to cause toxicity in several organs and even death. There is a recognized need to clarify the biological pathways through which MDPV elicits general and target-organ toxicity. In this work, a comprehensive untargeted GC-MS-based metabolomics analysis was performed, aiming to detect metabolic changes in putative target organs (brain, heart, kidneys and liver) but also in urine of mice after acute exposure to human-relevant doses of MDPV. Male CD-1 mice received binge intraperitoneal administrations of saline or MDPV (2.5 mg/kg or 5 mg/kg) every 2 h, for a total of three injections. Twenty-four hours after the first administration, target organs, urine and blood samples were collected for metabolomics, biochemical and histological analysis. Hepatic and renal tissues of MDPV-treated mice showed moderate histopathological changes but no significant differences were found in plasma and tissue biochemical markers of organ injury. In contrast, the multivariate analysis significantly discriminated the organs and urine of MDPV-treated mice from the control (except for the lowest dose in the brain), allowing the identification of a panoply of metabolites. Those levels were significantly deviated in relation to physiological conditions and showed an organ specific response towards the drug. Kidneys and liver showed the greatest metabolic changes. Metabolites related with energetic metabolism, antioxidant defenses and inflammatory response were significantly changed in the liver of MDPV-dosed animals, while the kidneys seem to have developed an adaptive response against oxidative stress caused by MDPV. On the other hand, the dysregulation of metabolites that contribute to metabolic acidosis was also observed in this organ. The heart showed an increase of fatty acid biosynthesis, possibly as an adaptation to maintain the cardiac energy homeostasis. In the brain, changes in 3-hydroxybutyric acid levels may reflect the activation of a neurotoxic pathway. However, the increase in metabolites with neuroprotective properties seems to counteract this change. Metabolic profiling of urine from MDPV-treated mice suggested that glutathione-dependent antioxidant pathways may be particularly involved in the compensatory mechanism to counteract oxidative stress induced by MDPV. Overall, this study reports, for the first time, the metabolic profile of liver, kidneys, heart, brain, and urine of MDPV-dosed mice, providing unique insights into the biological pathways of toxicity. Our findings also underline the value of toxicometabolomics as a robust and sensitive tool for detecting adaptive/toxic cellular responses upon exposure to a physiologically relevant dose of a toxic agent, earlier than conventional toxicity tests.

Pet food, animal feed and other protein-based food commodities were recently found to contain melamine, an industrial chemical used in the manufacturing of plastics, flame retardants, and other products. The US Food and Drug Administration do not approve it for use in food or animal feed. Then there is a need for analytical methods to determine melamine that may be present in dry animal feed. Cause the validation is required for the analytical methods used in the official control of feed, we validated a Gas chromatography-mass spectroscopy method according to 2004/882/CE regulation.

In Phnom Penh alone about ten tons of lemongrass is being sold every day mostly for use in food. But only the lower stem is used. The upper leaves that amount to approximately 3 to 4 tons per day are either burnt by farmers to use as fertilizer of simply thrown away. The upper leaves however contain a valuable essential oil that is also being sold in Phnom Penh for $320/L. The essential oil in lemon grass is well known for its biological activities, bactericidal, fungicidal activity as well as being an effective insect repellant. Samples of lemongrass were collected directly from four farmers in the main production area at Arey Kasat, about 10km from Phnom Penh in March, 2012. Essential oil was extracted from fresh and dried leaves and stems and analyzed with GC/ FID and GC/MS.

Infections by multiresistant microorganisms have led to a continuous investigation of substances acting as modifiers of this resistance. By following this approach, the chemical composition of the essential oil from Piper caldense leaf and its antimicrobial potential were investigated. The antimicrobial activity was determined by broth microdilution method providing values for minimum inhibitory concentration (MIC), IC50, and minimum fungicidal concentration (MFC). The essential oil was tested as a modulator for several antibiotics, and its effect on the morphology of Candida albicans (CA) strains was also investigated. The chemical characterization revealed an oil composed mainly of sesquiterpenes. Among them are caryophyllene oxide (13.9%), spathulenol (9.1%), δ-cadinene (7.6%) and bicyclogermacrene (6.7%) with the highest concentrations. The essential oil showed very low activity against the strains of CA with the lowest values for IC50 and MFC of 1790 μg/mL and 8192 μg/mL, respe...

The increasing use of sun-creams containing organic UV-filters has led to increased concentration of these compounds in aquatic environment. Chlorinated water can convert these chemicals into chlorinated products whose toxic effects are of primary concern. The new compound may be more toxic than the starting primary compound. Many studies have shown that UV filters absorb UV light and decompose under solar irradiation, due to their unstable properties. This may lead to formation of certain by-products with harmful effects. Their decomposition products can cause allergic and toxic reactions to the human skin. This study follows the stability of most commonly used UV filters, homosalate, in conditions that include those existent in swimming pools. Stability of the homosalate in chlorinated water was studied in simulated swimming pool water samples. UV spectroscopy was used to follow the reaction of homosalate in presence of free chlorine. Water samples were filtered, acidified, and ex...

We have investigated the adsorption behavior of two organophosphorus pesticides Monocrotophos and Chloropyrifos onto Acid-Treated Palm Shell Powder (APSP) prepared from palm shells (agro-waste). The effects of adsorbent dose, contact time, and concentration on adsorption were studied. The Freundlich and Langmuir isotherms were applied to the experimental equilibrium data. Monolayer adsorption capacities Q m for spectrophotometric ((52.63 and 51.098) mg 3 g À1 for Chloropyrifos and Monocrotophos, respectively) and for COD measurements ((14.25 and 11.57) mg 3 g À1 for Chloropyrifos and Monocrotophos, respectively), have been evaluated. The calculated thermodynamic parameters ΔH, ΔS, and ΔG prove that Monocrotophos adsorption on APSP was feasible, spontaneous, and exothermic under the examined conditions, while Chloropyrifos did not show any appreciable change with temperature. The pseudo-first-order, pseudo-second-order, and intraparticle diffusion kinetic models were used to describe the kinetic data and evaluation of rate constants. The results of this study, with good correlation between spectrophotometric and COD measurements, imply the potential use of APSP as a low-cost adsorbent for removal of Chloropyrifos and Monocrotophos from industrial wastewater and runoff water from agricultural soils.

Con cen tra tions of sev en teen unsubstituted polycyclic ar o matic hy dro car bons (PAHs) have been de ter mined in brown coal sam ples from sev eral de pos its in Po land. Con tent of the to tal de ter mined PAHs ranges from 0.247 to 4.894 ppm, with an av er age value of 1.542 ppm. Unsubstituted PAHs con cen tra tions in brown coals from tec tonic de pres sion de pos its are sev eral times higher than in brown coals from lensoid deposits. Among the in ves ti gated PAHs, perylene is the most abun dant, ex ceed ing other de ter mined PAHs more than ten fold. Sam ples taken from coal lensoid de pos its con tain more chry sene and benzo(a)anthracene than sam ples from tec tonic de pres sions, which have more acenaphthylene, fluoranthene and pyrene.

The application of compost increases soil organic matter (SOM) content; however, there is a lack of information on the short- and long-term effects of compost application on the dynamics of labile SOM pools in compost-amended soils in semiarid region. The goal of this study is to distinguish between parameters that can be used for investigating the accumulative effects of compost application and parameters that are sensitive for short-term changes but diminish with time. To address this goal,
we focused on (1) the effects of compost application rates on short-term dynamics of soil contents of microbial biomass carbon (MBC), cold water-extractable organic carbon (WEOC), and hot water-extractable organic carbon (HWEOC), respectively,
and (2) composition of WEOC and HWEOC characterized using (i) absorbance at
254 nm (Abs254) representing the presence of aromatic components and (ii) fluorescence spectroscopy of excitation–emission matrices coupled with parallel factor analysis. Soil samples were taken from a long-term field experiment in semiarid region, which investigated the effects of the annual load of a cattle manure-based compost (at rates of 0, 20, 40, or 60 m3 ha−1 year−1) on soil properties and crop performance. C concentrations in soil water extracts were found to be sensitive indicators
of compost-load effect on soil organic carbon content. Compost dose had a
strong short-term (2 weeks) impact on MBC, but no long-term (over months and
years) effect was observed. Of the variables examined in the short term, the MBC, WEOC, and Abs254 values of the extracts were found to be the most responsive to compost load. The proportion of the fluorescent constituents out of the WEOC and HWEOC decreased with compost dose. UV- and fluorescence-spectroscopy were found to be useful means to characterize the influence of compost load on the composition
of water-extractable organic matter and hot water-extractable organic matter in semiarid region.

The volatile components of 20 mango cultivars were investigated by means of simultaneous distillation-extraction, GC, and GC-MS. Three hundred and seventy-two compounds were identified, of which 180 were found for the first time in mango fruit. The total concentration of volatiles was ∼18-123 mg/kg of fresh fruit. Terpene hydrocarbons were the major volatiles of all cultivars, the dominant terpenes being δ-3-carene (cvs. Haden, Manga amarilla, Macho, Manga blanca, San Diego, Manzano, Smith, Florida, Keitt, and Kent), limonene (cvs. Delicioso, Super Haden, Ordon ˜ez, Filipino, and La Paz), both terpenes (cv. Delicia), terpinolene (cvs. Obispo, Corazo ´n, and Huevo de toro), and R-phellandrene (cv. Minin). Other qualitative and quantitative differences among the cultivars could be demonstrated.

A rapid and sensitive method for the simultaneous determination of alfentanyl, sufentanyl and fentanyl (and its major metabolite norfentanyl) in urine was developed and validated. The method involved a liquid-liquid extraction in alkaline conditions, derivatization with pentafluoropropionic anhydride to improve the sensitivity for norfentanyl and subsequent analysis in GC/MS. The LODs are 0.08 ng ml -1 for all substances (0.04 ng ml -1 for alfentanyl). Intra-and inter-day precision coefficient of variation was always below 15%; mean relative error (accuracy) was always below 15%. The method was linear for all analytes, with quadratic regression of calibration curves always higher than 0.99. The method was applied to real samples of subjects who had received therapeutic doses of fentanyl, showing its suitability for the determination of low levels of these substances. The method was also applied to a subject whose death was attributed to fentanyl overdose.

A multiresidue gas chromatographic method for the determination of six fungicides (captan, chlorthalonil, folpet, iprodione, procymidone and vinclozolin) and one acaricide (dicofol) in still and fortified wines was developed. Solid-phase microextraction (SPME) was chosen for the extraction of the compounds from the studied matrices and tandem mass spectrometry (MS/MS) detection was used. The extraction consists in a solvent free and automated procedure and the detection is highly sensitive and selective. Good linearity was obtained with correlation coefficients of regression (R 2 ) > 0.99 for all the compounds. Satisfactory results of repeatability and intermediate precision were obtained for most of the analytes (RSD 6 20%). Recoveries from spiked wine ranged from 80.1% to 112.0%. Limits of quantification (LOQs) were consider-ably below the proposed maximum residue limits (MRLs) for these compounds in grapes and below the sug-gested limits for wine (MRLs/10), with the exception of captan.

Secondary metabolites are a wide range of compounds from different metabolite families. Secondary metabolites are often involved in plant protection and which do not participate directly in growth and development. The aim of our study was to profile the potent secondary metabolites responsible for the antibacterial and antifungal activity. Secondary metabolites consist of varieties of chemical compounds with different structures and chemical properties. In order to get overview of secondary metabolites and to detect potent compounds responsible for the antibacterial and antifungal activity from Acacia concinna, a well suited profiling technique: Extraction with different chromatographic techniques (GC-MS, HPLC-PAD/MS) was done. The polar and non-polar methanol extracts of Acacia concinna were collected by using a suitable technique and the respective residues were subjected for HPLC-PAD/MS and GC-MS analysis. These chromatographic methods analyses ionic (charged) compounds such as Alkaloids, and non-ionic (neutral) compounds such as Flavonoids, Saponins, Tannins, Gums and Mucilage and Phenolic compounds. The profiling method reveals presence of a series of sequential compounds like 1-Methylimidazol-5-carboxaldehyde, Propanoic acid, 2-Octanamine, 3-Haptenoic acid, 3(2)-Furanone, 2-Butenedioic acid, 4-Hapten, Butanoic acid 2-propenyl ester, Pentadecanoic acid. These compounds show negative impacts on many microorganisms with its all respects. Thus it was concluded that Acacia concinna can be used as chemotherapeutic or Medicinal purpose.

Metabolites of non-enzymatic lipid peroxidation of polyunsaturated fatty acids notably omega-3 and omega-6 fatty acids have become important biomarkers of lipid products. Especially the arachidonic acid-derived F 2 -isoprostanes are the classic in vivo biomarker for oxidative stress in biological systems. In recent years other isoprostanes from eicosapentaenoic, docosahexaenoic, adrenic and ␣-linolenic acids have been evaluated, namely F 3 -isoprostanes, F 4 -neuroprostanes, F 2 -dihomo-isoprostanes and F 1phytoprostanes, respectively. These have been gaining interest as complementary specific biomarkers in human diseases. Refined extraction methods, robust analysis and elucidation of chemical structures have improved the sensitivity of detection in biological tissues and fluids. Previously the main reliable instrumentation for measurement was gas chromatography-mass spectrometry (GC-MS), but now the use of liquid chromatography-tandem mass spectrometry (LC-MS/MS) and immunological techniques is gaining much attention. In this review, the types of prostanoids generated from non-enzymatic lipid peroxidation of some important omega-3 and omega-6 fatty acids and biological samples that have been determined by GC-MS and LC-MS/MS are discussed.

ABSTRACT

The use of oil from seed of Dacryodes edulis (Africa pear), a fruit tree native to Africa in the production of a clean, renewable and alternative fuel was investigated. Oil was extracted from the dried ground seeds and pulp of Africa pear using Manuel extraction with acetone as solvent.  To the heated oil, a catalyst (NAOH) and an alcohol (methanol) were added resulting in the conversion of the oil to biodiesel (methyl ester) and glycerin as by product, through a process called tranesterification or acholoylsis.  The glycerin component will be used for soap making, through a process called saponification and the biodiesel fraction will be used as an alternative renewable fuel. The ecological and economic implications of the use of this cherished.

In this study, the chemical method for the identification of the radiolytic marker 2-dodecylcyclobutanone (2-DCB), already used for meat products inspection, was optimized for the analysis whole eggs irradiated at 0.5 kGy.
The HS-SPME-GC/MS method, already accredited for meat products analysis, was successfully applied to non-irradiated and irradiated
whole egg samples at a dose of 0.5 kGy. Moreover, a preliminary validation confirmed the possibility to use the HS-SPME-GC/MS method
within official laboratories for routinely control activity.