Combination of supported liquid membrane and solid-phase extraction for sample pretreatment of triazine herbicides in juice prior to capillary electrophoresis determination

A possibility of a combination of supported liquid membrane (SLM) and solid-phase extraction (SPE) for the determination of atrazine at microgram level in different type of fruit juices is presented. In comparison to SPE extraction from juice samples, the application of SLM-SPE enrichment provides much cleaner extracts and the possibility of lowering the limit of detection as low as 30 microg/l. However, it was also shown that by appropriate manipulation of SLM extraction conditions mainly flow-rate of donor phase and volume ratio between donor and acceptor phase, the level of detection can be further decreased to 10 microg/l. The results suggest that the application of SLM extraction prior…

Simultaneous determination of nine phytohormones in seaweed and algae extracts by HPLC-PDA.

An RP-HPLC-PDA method for the simultaneous analysis of 9 compounds deriving from the phytohormones class was developed and optimized, namely indoleacetic acid (IAA), indolebutyric acid (IBA), phenyleacetic acid (PAA), naphtyleacetic acid (NAA), trans-zeatin (TZ), kinetin (KA), isopentenyladenine (IA), 6-benzylaminopurine (6-BA) and abscisic acid (ABA). Validation of the method was performed on the SFE-CO2 extract made out of the mixture of Baltic algae. The regression coefficients for plant hormones were in the range from 0.997 to 0.999. The LOD and LOQ were on the levels from 0.05–0.29 and 0.15–0.88 mg/L, respectively. Developed method was used for the separation and determination plant ho…

Możliwości zastosowania ekstraktów roślinnych zawierających związki fenolowe w rolnictwie ekologicznym

Comparative Study of Different Column Types for the Separation of Polar Basic Hallucinogenic Alkaloids

The number of hallucinogenic compounds that have been separated simultaneously by liquid chromatography is limited. This research aimed to identify a column(s) that can allow for separation of several hallucinogens. The extent of separation of seven polar hallucinogenic tryptamine and phenethylamine derived alkaloids containing a basic N atom that becomes protonated at low pH values were investigated on five reverse-based columns and one hydrophilic interaction liquid chromatography (HILIC) column. An RP-phenyl and a negatively charged fused core HILIC were identified and recommended as effective columns in this regard. This research is the first to introduce a HILIC column in separation of…

Quantum and carbon dots conjugated molecularly imprinted polymers as advanced nanomaterials for selective recognition of analytes in environmental, food and biomedical applications

Abstract Samples with complex matrix analyzed during explanation of pathogenesis of various diseases and food or environmental monitoring request advanced analytical and instrumental devices. Among the materials used for described purposes, quantum (QDs) or carbon dots (CDs) layered by molecularly imprinted polymer (MIP) shells have gained widespread attention. Unique optical and physicochemical properties of QDs/CDs together with high MIPs selectivity make the QD/CD-MIP conjugates capable of adsorbing specific target molecules – such a binding event is then transduced as the optical signal of the response by the QDs/CDs. This review includes brief introduction on principles of imprinting p…

Pholiotina cyanopus, a rare fungus producing psychoactive tryptamines

Abstract Pholiotina cyanopus was collected from wood chips and other woody remnants of undetermined tree species. Its basidiomata were found in June within the area of closed sawmill in the central part of Żywiec city (SW Poland). Description and illustration of Ph. cyanopus based on Polish specimens are provided and its ecology, general distribution and comparison with similar taxa – Pholiotina smithii, Pholiotina sulcatipes, and others are discussed as well. The identity of the active compounds of Ph. cyanopus was additionally determined. Liquid chromatography–mass spectrometry (LC-MS) data sets were obtained to support the occurrence of psilocybin and its analogues – psilocin, baeocystin…

Peptides analysis in blood plasma using on-line system of supported liquid membrane and high-performance liquid chromatography

The potential of using supported liquid membrane (SLM) technique, combined with reversed-phase high-performance liquid chromatography (RP-HPLC) has been investigated for the determination of peptides in human blood plasma. The peptides studied were (DL)Leu(DL)Phe, MetLeuPhe, GlyLeuTyr and ValGluProlleProTyr. The carrier (Aliquat 336) was incorporated in membrane phase in order to facilitate the transport of investigated peptides. After extraction, the analyte-enriched acceptor phase was directly injected into an HPLC system for analysis. With SLM, high selectivity and efficiency were achieved for extraction of peptides in aqueous solutions. Lower extraction efficiency was obtained in plasma…

Mode of action of herbicidal derivatives of aminomethylenebisphosphonic acid. I. Physiologic activity and inhibition of anthocyanin biosynthesis

N-Pyridylaminomethylenebisphosphonic acids constitute a class of promising herbicides. Since their mode of action at the cellular level is still poorly understood, we studied the influence of N-pyridylaminomethylenebisphosphonic acids on plant growth, at the whole plant and undifferentiated tissue levels, using seedlings and cell suspension cultures of mono- and dicotyledonous species. These compounds exhibited strong herbicidal properties, being equipotent with the popular herbicide glyphosate. Since they also depressed buckweed anthocyanin biosynthesis, the shikimate pathway could represent a site of action of N-pyridylaminomethylenebisphosphonic acids.

The Biomass of Algae and Algal Extracts in Agricultural Production

Fertilizers and plant growth regulators (PGRs) based on seaweeds are commonly known, having been produced and utilized for dozens of years. Algae are rich in carbohydrates, proteins, minerals and chemical compounds that belong mainly to the following groups: polysaccharides, polyphenols, phlorotannins, plant pigments, unsaturated fatty acids, sterols and plant hormones.

Spectral characteristics of 5-hydroxymethylfurfural as a related substance in medicinal products containing glucose

Objectives: To study 5-hydroxymethylfurfural (5-HMF) spectral characteristics aiming at their future application in analytical procedures and their validation for the determination of 5-HMF in liquid products containing glucose after sterilization.Method: Direct spectrophotometric method for the determination of 5-HMF using the molar absorption coefficient at the absorption maximum (284 nm).Results and discussion: aqueous 5-HMF solutions have strong absorption in the ultraviolet range below 310 nm and give two absorption maxima at wavelengths of 229–230 nm and 284 nm. An excellent linear relationship between absorbance and 5-HMF concentration was observed in the concentration range of 2.0–1…

EFFECT OF SURFACTANT AND SUBSTRATE TEMPERATURE ON THE GROWTH OF Ag FILMS ON A SAPPHIRE SURFACE

The possibility of modification of the thin film growth on an insulating (sapphire) substrate by using a Ga monolayer as a "surfactant" was studied. We found that the films grown in this way are electrically conducting and can emit photoelectrons at much lower thickness than those deposited on a pure substrate. The surfactant stabilizes the positions of Ag atoms on the substrate surface and inhibits the coalescence of small nuclei into bigger islands, even when the film is annealed to 450 K. This fact may be very important for thin metal film technology.

Theoretical and experimental NMR studies on muscimol from fly agaric mushroom (Amanita muscaria)

In this article we report results of combined theoretical and experimental NMR studies on muscimol, the bioactive alkaloid from fly agaric mushroom (Amanita muscaria). The assignment of (1)H and (13)C NMR spectra of muscimol in DMSO-d6 was supported by additional two-dimensional heteronuclear correlated spectra (2D NMR) and gauge independent atomic orbital (GIAO) NMR calculations using density functional theory (DFT). The effect of solvent in theoretical calculations was included via polarized continuum model (PCM) and the hybrid three-parameter B3LYP density functional in combination with 6-311++G(3df,2pd) basis set enabled calculation of reliable structures of non-ionized (neutral) molecu…

Photoelectron spectroscopy of thin discontinuous metal films deposited onto a sapphire substrate

Abstract The charging of small metallic clusters forming discontinuous gold and gallium films, condensed in vacuum onto an insulating substrate (sapphire), was experimentally studied by the method of ultraviolet photoelectron spectroscopy (UPS) for a photon energy of 5.4 eV. It seems that the charging is due to electron emission as well as to electron transfer from metal islands to the empty electron states in the metal-insulator interface.

Direct Analysis of Psilocin and Muscimol in Urine Samples Using Single Drop Microextraction Technique In-Line with Capillary Electrophoresis

The fully automated system of single drop microextraction coupled with capillary electrophoresis (SDME-CE) was developed for in-line preconcentration and determination of muscimol (MUS) and psilocin (PSC) from urine samples. Those two analytes are characteristic active metabolites of Amanita and Psilocybe mushrooms, evoking visual and auditory hallucinations. Study analytes were selectively extracted from the donor phase (urine samples, pH 4) into the organic phase (a drop of octanol layer), and re-extracted to the acidic acceptor (background electrolyte, BGE), consisting of 25 mM phosphate buffer (pH 3). The optimized conditions for the extraction procedure of a 200 &micro

Supported liquid membrane extraction of glyphosate metabolites

Use of the supported liquid membrane (SLM) technique for (aminomethyl)phosphonic acid (AMPA) extraction is presented. For the extraction of this analyte a suitable SLM system involves a liquid membrane containing Aliquat 336 – a cationic carrier that facilitates AMPA transport. The extraction of this compound, as in the case of glyphosate, is dependent on the donor phase pH and the concentration and type of counter-ion in the acceptor phase, although some differences are also observed. In both cases the transport mechanism is counter-coupled transport in which the driving force of mass transport over the membrane is created by the gradient of chloride anions from the acceptor to donor phase.

Biowęgiel jako środek polepszający właściwości gleby

Stereoselective synthesis of 2-amino-1-hydroxy-3-phenylpropylphosphonic acid

Abstract A highly stereoselective synthesis of 2-amino-1-hydroxy-3-phenylpropylphosphonic acid was achieved by simple addition of diethyl phosphite to enantiomeric N-blocked phenylalaninals. These compouds exhibit significant herbicidal activity.

Chromatographic profiles and antimicrobial activity of the essential oils obtained from some species and cultivars of the Mentheae tribe (Lamiaceae)

Abstract The present study was focused on the chemical composition and antimicrobial activity of the essential oils (EsO) obtained from five Lamiaceae representatives grown in the south of Ukraine. Among them are Salvia sclarea L., Monarda didyma (cultivar ‘Cambridge Scarlet’), Thymus pulegioides (cultivar ‘2/6-07’), Thymus vulgaris (cultivar ‘Jalos’), and Thymus serpyllum L. The component analysis of the EsO was carried out by gas chromatography method coupled with mass spectrometry (GC–MS). The antimicrobial properties of the EsO were determined using the agar diffusion test against widespread pathogenic bacterial strains (Staphylococcus aureus, Escherichia coli, Enterococcus faecalis, St…

Introduction to MIP synthesis, characteristics and analytical application

Abstract One of the trends in analytical chemistry is associated with designing and developing new types of sample preparation techniques, which might significantly increase the efficiency and selectivity of the analytes isolation or/and preconcentration process. One of the most widely employed solutions is selective sorption materials, defined as molecularly imprinted polymers (MIPs), as well as the sorbents with the molecular fingerprint. Due to their simple preparation protocol, mechanical, thermal and chemical stability and selectivity, MIPs have found application as a stationary phase in separation techniques such as liquid chromatography or capillary electrophoresis, in electrochemica…

Extraction of glyphosate by a supported liquid membrane technique.

The possible application of the supported liquid membrane (SLM) technique for the extraction of glyphosate is presented. For the extraction of this compound the SLM system has been applied with utilisation of Aliquat 336 as a cationic carrier incorporated into the membrane phase. The extraction efficiency of glyphosate [N-(phosphonomethyl)glycine] is dependent on the donor phase pH, carrier concentration in the organic phase and NaCl concentration in the acceptor phase. The optimal extraction conditions are: donor phase pH>11, acceptor phase of 2 M NaCl solution and the organic phase composed of 20% (w/w) Aliquot 336 solution in di-hexyl ether. Counter-coupled transport of chloride anions f…

Chemical Composition of Two Different Lavender Essential Oils and Their Effect on Facial Skin Microbiota

Lavender oil is one of the most valuable aromatherapy oils, its anti-bacterial and anti-fungal activities can be explained by main components such as linalool, linalyl acetate, lavandulol, geraniol, or eucalyptol. The aim of the study was to assess the anti-microbial effects of two different lavender oils on a mixed microbiota from facial skin. The commercial lavender oil and essential lavender oil from the Crimean Peninsula, whose chemical composition and activity are yet to be published, were used. Both oils were analysed by gas chromatography coupled to mass spectrometry. The composition and properties of studied oils were significantly different. The commercial ETJA lavender oil contain…

Chemical Composition of Herbal Macerates and Corresponding Commercial Essential Oils and Their Effect on Bacteria Escherichia coli

This study addresses the chemical composition of some commercial essential oils (clove, juniper, oregano, and marjoram oils), as well as appropriate herbal extracts obtained in the process of cold maceration and their biological activity against selected Escherichia coli strains: E. coli ATTC 25922, E. coli ATTC 10536, and E. coli 127 isolated from poultry waste. On the basis of the gas chromatography-mass spectrometry (GCMS) analysis, it was found that the commercial essential oils revealed considerable differences in terms of the composition and diversity of terpenes, terpenoids and sesquiterpenes as compared with the extracts obtained from plant material. The commercial clove, oregano, a…

Herbicidal activity of derivatives of 9-aminofluoren-9-ylphosphonic acid

A series of derivatives of 9‐aminofluoren‐9‐ylphosphonic acid (phosphonic analogues of morphactins) were synthesized and screened for herbicidal activity against Lepidium sativum, Cucumis sativus and Lycopersicon esculentum. Ethyl 9‐(N‐alkylamino)fluoren‐9‐yl(phenyl)phosphinates appeared to be equipotent with glyphosate and thus may be recognized as new lead compounds for further structural modifications.

The application of the supported liquid membrane and molecularly imprinted polymers as solid acceptor phase for selective extraction of biochanin A from urine

An efficient sample clean-up and preconcentration procedure for phytoestrogens analysis in urine has been developed. It was based on a combination of solid phase extraction with hollow-fiber supported liquid membrane and molecularly imprinted beads (MIPs-HF-SLM-SPE). The molecularly imprinted polymers (MIPs) were synthesized by precipitation polymerization technique with biochanin A (BCA) as a template, giving narrowly dispersed microspheres with a regular shape. As the functional monomer, (dimethylamino)ethyl methacrylate (-DEM) turned out to be better than methacrylic acid (MAA) to get the best-imprinted effects. The MIPs used as sorbents in the MIPs-HF-SLM-SPE extraction process exhibite…

Supercritical Algal Extracts: A Source of Biologically Active Compounds from Nature

The paper discusses the potential applicability of the process of supercritical fluid extraction (SFE) in the production of algal extracts with the consideration of the process conditions and yields. State of the art in the research on solvent-free isolation of biologically active compounds from the biomass of algae was presented. Various aspects related with the properties of useful compounds found in cells of microalgae and macroalgae were discussed, including their potential applications as the natural components of plant protection products (biostimulants and bioregulators), dietary feed and food supplements, and pharmaceuticals. Analytical methods of determination of the natural compou…

Single hollow fiber SLM extraction of polyamines followed by tosyl chloride derivatization and HPLC determination

Determination of polyamines in biological fluids possesses medical diagnostic relevance. Despite the vast panel of analytical methods developed for polyamines they are not applied in routine clinical usage, mainly due to the time and labor consuming sample preparation step and complicated derivatization procedures. Thus, new simpler methods are needed. This paper describes a single hollow fiber SLM extraction method of polyamines followed by simple pre-column derivatization with tosyl chloride and HPLC-UV analysis. The influence of different parameters such as the extraction time, organic phase composition, acceptor pH, donor pH, acceptor volume, donor volume and stirring speed on the trans…

Supported liquid membrane extraction of aromatic aminophosphonates

Abstract A fast and efficient supported liquid membrane (SLM) extraction system for the series of substituted aromatic aminophosphonates was elaborated. The mass transfer of solute was examined in terms of operator (pH and ionic strength of water phase, composition of membrane phase and the concentration of analyte) dependent parameters. Additionally, the influence of the aminophosphonates structure on the extraction efficiency was examined. From the results it can be concluded that the most effective conditions of membrane process are 10% (w/w) carrier concentration (Aliquat 336) in the liquid membrane, high pH of donor phase (pH=11) and moderate salt concentration (0.4 M NaCl) in the acce…

Continuous flow synthesis of amine oxides by oxidation of tertiary amines

The synthesis of N-methylmorpholine N-oxide by oxidation of N-methylmorpholine with hydrogen peroxide was implemented in a microstructured reactor for increased safety and larger-scale applications. The active oxidant, peroxymonocarbonate HCO4− is formed in situ from the equilibrium reaction of hydrogen peroxide and bicarbonate. The bicarbonate can be induced by hydration of carbon dioxide. Elaborate studies on the influence of the catalyst concentration and temperature were carried out and the observed activation energy was determined. Elevated temperatures up to 60 °C and a carbon dioxide concentrations of 1 wt% led to a conversion for N-methylmorpholine of approximately 98% within 13.90 …

Studies of polyamines transport through liquid membranes with D2EHPA as a carrier.

The transport of polyamines through the liquid membranes with di‐2‐ethylhexyl phosphoric acid (D2EHPA) was investigated. The study was performed in three main steps: liquid–liquid extraction (LLE), bulk liquid membrane (BLM) extraction, and supported liquid membrane (SLM) extraction. Equilibrium distribution experiments allowed determining the extraction constants and stoichiometric coefficients for each polyamine. It turned out that one amino group binds two molecules of carrier (one D2EHPA dimer) and the extractability of polyamine rises with the increase in number of function groups in the molecule. The BLM and SLM experiments showed that despite considerable differences in distribution …

Molecular Fingerprints of Thyroid Cancer Cells by Using Library of Molecular Receptors Formed by N-Lipidated Peptides Immobilized on Cellulose

This paper presents a novel diagnostic method using a library of molecular receptors to assess the composition of healthy and tumorous tissue samples. Molecular receptors were formed by self-organization of N-lipidated peptides attached in the regular fashion via aminophenylamino-1,3,5-triazine linkers to the surface of a cellulose plate. The library was cloned into multiple, identical copies. A new clone was used in each test. The binding process was monitored by staining the discs with Brilliant Black and quantitative color measure- ment was performed in 256-grade grayscale. Substantial differences in the composition of healthy and tumor samples were observed in most cases. The sharp diff…

Chromatographic Profiles of the main Secondary Metabolites in the Monarda fistulosa L. Aerial Part

Two different methods of chromatographic analysis have been used in this study for the phytochemical evaluation of main secondary metabolites in the aerial part of bee balm (Monarda fistulosa L.) as the non-officinal medicinal plant of the Lamiaceae Martinov family. The high performance thin layer chromatography (HPTLC) fingerprinting method was developed for the qualitative analyses of phenolic and non-polar compounds in the bee balm herb after its maceration in the solvents of different polarity. Such polyphenols as rosmarinic, caffeic and chlorogenic acids were authentically identified in the methanol extract of herb using HPTLC. Aromatic monoterpenoid thymol was identified by the HPTLC …

Transport mechanism of peptides through supported liquid membranes

Abstract The transport of selected dipeptides through supported liquid membranes impregnated with di(2-ethylhexyl) phosphoric acid in n-dihexylether has been investigated. The fluxes depend on the side chain of amino acids, presence in the peptide structure. The highest fluxes were obtained for the peptides extracted with the highest efficiency. It has been found that the hydrophobicity of investigated peptides, was not the major factor, influences their SLM permeation. In the conditions studied, it has been observed that the transport of peptide–carrier complex was depending on the acidic–basic properties of the analyte. The linearly least-square fittings of log {K1 + [H+]D} and log[(HR)2]…

Development of high-performance thin layer chromatography method for identification of phenolic compounds and quantification of rosmarinic acid content in some species of the Lamiaceae family

ABSTRACT Aim: Representatives of Nepetoideae Burnett subfamily are promising species of the Lamiaceae Martinov family because of accumulating such valuable groups of secondary metabolites as terpenoids and polyphenols. A high-performance thin layer chromatography (HPTLC) fingerprint method for the qualitative determination of phenolic compounds and for the quantification of rosmarinic acid (RA) content in methanol extracts of five species of this subfamily was developed for the first time. Materials and Methods: Dried aerial parts of Dracocephalum moldavica L., Ocimum americanum L., Lophanthus anisatus (Nutt.) Benth., Monarda fistulosa L., and Satureja hortensis L. collected in flowering pe…

Supercritical fluid extraction of algae enhances levels of biologically active compounds promoting plant growth

The aim of this research was to screen plant growth biostimulant properties of supercritical CO2 macroalgal extracts. To this end secondary metabolites were isolated from the biomass of marine macroalgae from the Baltic Sea (species of Polysiphonia, Ulva and Cladophora). Chemical characteristics of the algal extracts were determined by inductively coupled plasma atomic emission spectroscopy for inorganic constituents and high-performance liquid chromatography and spectrophotometry for organic constituents. Inorganic (macro- and microelements) and organic (plant hormones: auxins and cytokinins; polyphenols) compounds were detected in the extract. Algal extracts were tested primarily on garde…

Rapid determination of ibotenic acid and muscimol in human urine

The preparation and evaluation of core-shell magnetic dummy-template molecularly imprinted polymers for preliminary recognition of the low-mass polybrominated diphenyl ethers from aqueous solutions

Abstract The design, preparation process, binding abilities, morphological characteristic and prospective field of application of dummy-template magnetic molecularly imprinted polymer (DMMIP) for preliminary recognition of the selected low-mass polybrominated diphenyl ethers (PBDE-47 and PBDE-99) from aquatic environment were investigated. The surface of iron oxide (Fe3O4) nanopowder (50–100 nm particles size) was modified with tetraethoxysilane and next prepared Fe3O4@SiO2 particles were dispersed in anhydrous toluene functionalized by (3-aminopropyl)triethoxysilane. Finally, MIPs' thin film layer on the surface of Fe3O4@SiO2@NH2 was formed in acetonitrile as a solvent solution, using ethy…

Factors influencing the transport of tryptophan hydrochloride through supported liquid membranes containing macrocyclic carriers

Commercially available PTFE membranes were used as a support for liquid membranes in amino acid transport. Using tryptophan as a model amino acid, the influence of the type of organic liquid, kind of macrocyclic carrier and counter-ion on transport efficiency was examined. These studies show the strong influence of the kind of the counter-ion co-transported with amino acid cation, and the type of macrocyclic carrier used on the transport efficiency. The transport efficiency depends also on the pH of the source phase and on the nature of the organic liquid used as a membrane solvent. Liquid membranes supported on commercial porous-PTFE-membranes with hydrophobic solvents are stable for more …

Approach of the State Pharmacopeia of Ukraine to analytical procedures validation on the example of chloride ions assay in peritoneal dialysis solutions

The objective of this study was to develop and validate an alternative analytical procedure for the total chloride assay in solutions for peritoneal dialysis (PD). The proposed analytical procedure was validated according to the requirements of the International Conference on Harmonization (ICH) Guideline: Topic ICH Q2(R1) and the approach of the State Pharmacopeia of Ukraine (SPU). The analytical procedure was specific. The li-nearity of the procedure was evaluated in the concentration range of 76 to 114 mmol/L of chloride ions (80-120% of the stated content (95 mmol/L)) with the regression equation y = 1.0029 ∑ X -0.2269 and a correlation coefficient of 0.9989. The y-intercept of the regr…

Determination of glyphosate and aminomethylphosphonic acid in natural water using the capillary electrophoresis combined with enrichment step

A previously elaborated capillary electrophoresis (CE) method used for the determination of glyphosate and aminomethylphosphonic acid (AMPA) was slightly modified in order to improve the sensitivity. However, detection limits attained (5 μg mL−1 for glyphosate and 4 μg mL−1 for AMPA) were still not satisfactory for analytical purposes, thus the addition of a preconcentration step before the CE analysis was proposed. AMBERLITE®IRA-900, a strong anion-exchange resin, was used to preconcentrate both analytes in environmental aqueous samples. The experimental conditions optimised in a previous work were readapted, by decreasing the eluent concentration due to CE limitations. Satisfactory result…

Plant-growth-regulating phosphono peptides

Phosphono peptides exhibited plant‐growth‐regulating activity when tested on Lepidium sativum and Cucumis sativus. The studies have provided evidence that the mechanism of action of these compounds may involve the uptake of the phosphono peptides into the plant, intracellular hydrolysis of the peptide bond and release of the P‐terminal aminoalkylphosphonic acid. This acid or its metabolite is then probably responsible for the observed physiological effect.

Sedative Effect and Standardization Parameters of Herbal Medicinal Product Obtained from the Ocimum americanum L. Herb

Abstract Sedative phytomedications continue to play an important role in the management of a considerable amount of anxiety symptoms because of the various side effects of synthetic sedatives and tranquilizers. However, developing new herbal drugs needs their appropriate quality control according to the relevant requirements. The aim of the study was to determine the sedative properties of the tinctures obtained from the American basil (Ocimum americanum L., Lamiaceae Martinov family) herb and to develop the standardization parameters for the promising herbal medicinal product. The open field test was used to evaluate the sedative effect of the prepared tinctures: (1) with the added of O. a…

Transport of amino acids and their phosphonic acid analogues through supported liquid membranes containing macrocyclic carriers. Experimental parameters

Abstract Amino acid hydrochlorides are well transported through 1-decanol membranes containing Kryptofix 5 or 222 and supported in a porous polyacrylonitrile hollow fiber matrix. Factors which influence the transport of phenylalanine hydrochloride were studied in some detail using this sheet- as well as hollow fibre-supported liquid membranes. These studies show that the choice of the membrane phase, the kind of polymeric support and the mode of membrane preparation are of great importance for the efficiency of the process. The most vital step in the membrane preparation appears to be its activation by soaking in a solution of phenylalanine hydrochloride in a water-ethanol or water-propanol…

Enrichment of amino acids by supported liquid membrane extraction using Aliquat 336 as a carrier

Abstract The possible application of Aliquat 336 (trioctylmethyl ammonium chloride) as a carrier for liquid membrane extraction of amino acids was investigated. The extraction is performed from an aqueous donor phase with pH > 11 to an acceptor phase containing a salt solution through a supported liquid membrane with Aliquat 336 as a carrier in the membrane to facilitate amino acid transport. Counter-coupled transport of chloride anions from the acceptor phase to the donor phase is the driving force of the mass transfer in this system. The extraction efficiency depends on the donor phase pH, the carrier concentration in the liquid membrane, the composition of the acceptor phase and the hydr…

Enantiodifferentiation of N-benzyloxycarbonylaminophosphonic and phosphinic acids and their esters using cyclodextrins by means of capillary electrophoresis

Capillary electrophoresis was successfully applied for separation of the enantiomers of N-benzyloxycarbonyl-alpha-aminophosphonic and alpha-aminophosphinic acids as well as their ethyl and phenyl monoesters with the use of a range of commercially available cyclodextrins (alpha, beta and hydroxypropyl-gamma-cyclodextrins) as chiral selectors. The dependence of effectiveness of separation on type and concentration of these chiral selectors as well as on pH of background electrolyte was examined in some detail.

Characterization of particle morphology of biochanin A molecularly imprinted polymers and their properties as a potential sorbent for solid-phase extraction

Abstract Molecularly imprinted polymers (MIPs) with biochanin A as a template were obtained using a bulk polymerization with non-covalent imprinting approach. The polymers were prepared in acetonitrile as porogen, using ethylene glycol dimethacrylate (EDMA) as cross-linking agent. The synthesis, with an application of 1′,1′-azobis(cyclohexanecarbonitrile) (ACHN) as an initiator, has been performed thermally. During the synthesis process the effect of different functional monomers such as methacrylic acid (MAA), acrylamide (AA) and 4-vinylpyridine (4-VP) was investigated. The application of nitrogen sorption porosimetry, scanning electron microscopy (SEM), and Fourier transform infrared spec…

Synthesis of peptides with α,β‐dehydroamino acids, I. synthesis of N‐benzyloxycarbonyl and N‐trifluoroacetyl dipeptides of dehydroalanine and dehydrophenylalanine

Condensation of amides of N-(benzyloxycarbonyl)- and N-(trifluoroacetyl)amino acid with pyruvic and phenylpyruvic acid yields, in the presence of p-toluenesulfonic acid as a catalyst, N-(benzyloxycarbonyl)- and N-(trifluoroacetyl)dehydro dipeptides with C-terminal Δ Ala and ΔPhe, respectively (Table 2 and 3). Synthese von Peptiden mit α,β-Dehydroaminosauren, I. - Synthese von N-(Benzyloxycarbonyl)-und N-(Trifluoracetyl) dipeptiden von Dehydroalanin und Dehydrophenylalanin Die Kondensation von Nα-(Benzyloxycarbonyl)- und Nα-(Trifluoracetyl)aminosaureamiden mit Brenztrauben- und Phenylbrenztraubensaure in Gegenwart von p-Toluolsulfonsaure als Katalysator fuhrt zu N-(Benzyloxycarbonyl)- und N-…

Antioxidant Phenolic Compounds in Salvia officinalis L. and Salvia sclarea L.

Abstract The differences in the chemical composition of the phenolic compounds of Salvia officinalis versus Salvia sclarea growing in different habitats, were studied. First, the optimal solvent - methanol - for ultrasonic extraction of phenolic compounds from these plants was chosen experimentally. Total phenolic content and 1,1-diphenyl-2-picrylhydrazyl (DPPH) assays were determined spectrophotometrically. Total phenolic content was in the range of 63.9 to 134.4 mg GAE/g of plant depending on the studied species. The highest antiradical activity was displayed by the methanol fractions of S. sclarea varieties (83 and 67%). HPLC-DAD analysis of extracts was done in order to identify the pre…

Crown-ether mediated transport of amino acids through an immobilized liquid membrane

Application of Molecular Imprinted Polymers for Selective Solid Phase Extraction of Bisphenol A

Abstract Selective molecularly imprinted polymers (MIPs) with bisphenol A as template were synthesized using the non-covalent imprinting approach. MIPs were prepared using thermally initiated polymerization with 1,1’-azobis(cyclohexanecarbonitryle) (ACHN) as initiator and ethylene glycol dimethacrylate (EDMA) as a cross-linking agent. The tested functional monomers included methacrylic acid, acrylamide, and 4-vinylpyridine. The selectivity of the BPA-MIP for the solid phase extraction of bisphenol A was tested in samples containing other related alkylphenols. The polymers prepared in acetonitrile using methacrylic acid or acrylamide as monomer showed the highest selectivity towards target a…

The Influence of Chemical Composition of Commercial Lemon Essential Oils on the Growth of Candida Strains

Candida yeasts are saprophytes naturally present in the environment and forming colonies on human mucous membranes and skin. They are opportunistic fungi that cause severe and even fatal infections in immunocompromised individuals. Several essential oils, including eucalyptus, pine, cinnamon and lemon, have been shown to be effective against Candida strains. This study addresses the chemical composition of some commercial lemon essential oils and their antifungal potential against selected Candida yeast strains. Antifungal potential and minimum inhibitory concentrations were determined for six commercial lemon essential oils against five Candida yeast strains (Candida albicans 31, Candida t…

Chronic kidney disease and dialysis therapy: incidence and prevalence in the world

Сhronic kidney disease (CKD) is the important public and medical problem in the world because of a large burden on health care systems. The prevalence of CKD and number of dialysis patients are increasing in the world. The prevalence and incidence of CKD depends on age, race, and gender of patients, region, and the presence of the CKD registry in a country. Diabetes mellitus (DM) and arterial hypertension (AH) are the most common causes of end stage renal disease (ESRD). It is projected that the number of dialysis patients will reach 5.5 million in 2030. Specific strategies and interventions should be urgently aimed at reducing in the burden of CKD by means of the prevention, detection and …

Determination of glyphosate and its metabolite aminomethylphosphonic acid in fruit juices using supported-liquid membrane preconcentration method with high-performance liquid chromatography and UV detection after derivatization with p-toluenesulphonyl chloride

Abstract The application of supported-liquid membrane (SLM) technique for effective extraction of N -(phosphonomethyl)glycine (glyphosate) and its primary metabolite aminomethylphosphonic acid (AMPA) from juices (orange, grapefruit, apple and blackcurrant) in combination with HPLC-UV detection after derivatization with p -toluenesulphonyl chloride (TsCl) is presented. The influence of various parameters such as the composition of acceptor phase, flow-rate, concentration of analytes, on the performance of extraction procedure, was studied. It was shown that by appropriate manipulation of SLM parameters the level of detection could be significantly improved. The influence of SLM conditions on…

Supported liquid membrane separation of amine and amino acid derivatives with chiral esters of phosphoric acids as carriers

Studies on the possible use of phosphate and phosphonate esters bearing chiral menthol or nopol moieties as carriers for the transport of amines, amino acids, and amino acid esters through supported liquid membranes (SLM) are presented. Additionally, the enantioselectivity of the SLM transport of alkyl esters of aromatic amino acids and a non‐protein amino acid was also evaluated. It could be concluded that the extent of transport strongly depends on the hydrophobicity of the amino compound. Moreover, the carrier structure also influences the transport of those compounds through SLM: chiral phosphate and phosphonate esters appear to be poor or moderate carriers for enantioselective SLM tran…

Isolation and determination of phenolic compounds from freshwater Cladophora glomerata

Abstract Marine algae biomass has gained widespread interest in the world of science and many industries. The growing number of publications proves that these algae are an interesting and essential natural resource. This interest is due to the presence of a variety of biologically active compounds that give algae extracts a broad spectrum of biological and functional properties. However, there is little data on the chemical composition of algae obtained from freshwater. This work focuses on the isolation and determination of phenolic compounds from freshwater algae of the species Cladophora glomerata. Different types of extraction and extractants were used to isolate these bioactive compoun…

The ability of soil-borne fungi to degrade organophosphonate carbon-to-phosphorus bonds

The ability of a wide variety of soil-borne fungal strains to degrade four structurally different compounds containing P-C bonds, namely the naturally occurring amino acid ciliatine, the popular herbicide glyphosate, phosphonoacetic acid and 2-amino-3-phosphonopropionic acid, was studied in order to show that soil fungi may play an important role in the biodegradation of organophosphonates. Most of the strains appeared to utilize ciliatine as the sole source of phosphorus for growth. Only a limited number of strains were able to grow on the other phosphonates used in this work. The strains of Trichoderma harzianum, Scopulariopsis sp. and Aspergillus niger chosen for more detailed study show…

Computational modeling of molecularly imprinted polymers as a green approach to the development of novel analytical sorbents

Abstract The development of novel molecularly imprinted polymers (MIP) sorbents for specific chemical compounds require a lot of tedious and time-consuming laboratory work. Significant quantities of solvents and reagents are consumed in the course of the verification of appropriate configurations of polymerization reagents. Implementation of molecular modeling in the MIP sorbent development process appears to provide a solution to this problem. Appropriate simulations and computations facilitate the determination of the nature of interaction between the reagents and thus the selection of the best configuration of chemicals for the preparation of the sorbent. The article presents literature …

Oxidation of secondary alcohols by duckweed: A biotransformation experiment for undergraduate students

New adsorbents for thymidylate synthase affinity chromatography

New affinity adsorbents, intended for chromatography of thymidylate synthase (EC 2.1.1.45) from different sources, consisting of p-[N-[(2-amino-4-hydroxy-6-quinazolinyl)-methyl]-N-2-propynylamino]benzoyl-γ-[α-(3-carboxypropylamino)]glutamyl-glutamyl immobilized either on macroporous copolymer of acrylonitrile and n-butyl acrylate or on macroporous polymer of acrylonitrile itself, both crosslinked with divinylbenzene and having aminoethyl groups, were obtained. Both adsorbents were found to be effective in dUMP-dependent binding of thymidylate synthase from regenerating rat liver.

Synthesis and herbicidal activity of isoxazole-substituted 1-aminoethylphosphonates and 1-hydroxyethylphosphonates

Isoxazole‐substituted 1‐aminoethyl‐ and 1‐hydroxyethyiphosphonates were synthesized by a multi‐step procedure and were screened for herbicidal activity against Lepidium sativum L. and Cucumis sativus L. All the synthesized compounds exhibited notable herbicidal activity.

ChemInform Abstract: Stereoselective Synthesis of 2-Amino-1-hydroxy-3- phenylpropylphosphonic Acid.

Abstract A highly stereoselective synthesis of 2-amino-1-hydroxy-3-phenylpropylphosphonic acid was achieved by simple addition of diethyl phosphite to enantiomeric N-blocked phenylalaninals. These compouds exhibit significant herbicidal activity.

Complex technological and biological research of solutions for peritoneal dialysis

Objective : The purpose of our work was to conduct technological, analytical, and biological investigations and stability studies of peritoneal dialysis (PD) solutions containing glucose and sodium lactate in single-chamber containers. Methods : Different formulations of PD solutions were prepared and sterilized at a temperature of 121 °C during 15 m. UV-spectrophotometric determination was performed using purified water as a blank. The spectra of the solutions were run in the range of 220 to 400 nm for the identification of an absorption maximum (λ max ) and measuring the absorbance at 228-230 nm and λ max before and after heat sterilization. λ max of the most PD solutions after sterilizat…

Interaction of sodium, lithium, caesium, and potassium ions with ascorbyl radicals.

Abstract The influence of the concentration of sodium, lithium , caesium, and potassium ions as well as of the ionic strength of the solutions used on the dismutation rate of ascorbyl radicals has been investigated. While the dismutation rate was not influenced by Li+, it decreased, however, with increasing concentrations of the other ions investigated. The largest effect was obtained with Na+. This change in dismutation rate indicates a stabilizing effect on ascorbyl radical by these ions.

Influence of temperature on mass transfer in an incomplete trapping single hollow fibre supported liquid membrane extraction of triazole fungicides.

The influence of temperature in a single hollow fibre supported liquid membrane extraction of triazole fungicides with a stagnant acceptor phase was investigated. The mass transfer parameters such as diffusion coefficient, flux and apparent viscosity were determined at temperature ranging from 278 K to 313 K. Increase in temperature led to an increase in diffusion coefficient and flux. The apparent viscosity also decreased with an increase in temperature. The degree of trapping in the acceptor phase influenced the mass transfer at higher temperature. At lower temperature, the transport of analytes from the donor solution through the donor-membrane interface and through the membrane mainly a…

Separation of amino acid enantiomers using supported liquid membrane extraction with chiral phosphates and phosphonates

A series of dialkyl and monoalkyl phosphates, phosphites and phosphinates based on (−)-menthol and (−)-nopol were synthesized and used as carriers for transport of aromatic amino acids through supported liquid membranes. Although all the compounds were found to be effective carriers (with transport rate dependent on their structure) the enantioselectivity of the process obtained was low or moderate. Aromatic amino acids were enantioselectively transported through supported liquid membranes containing chiral phosphates, phosphites and phosphinates as carriers. Download full-size image

Mode of action of herbicidal derivatives of aminomethylenebisphosphonic acid. Part II. Reversal of herbicidal action by aromatic amino acids

The herbicidal action of N-pyridylaminomethylenebisphosphonic acids is accompanied by an impairment of anthocyanin biosynthesis. This suggests that they might act as inhibitors of some steps in aromatic amino acid biosynthesis. Herbicidal effects were reversed by aromatic amino acids using both bacterial and plant models, a finding that strongly supports this hypothesis. Structural features of these compounds suggest the sixth enzyme in the shikimate pathway 5-enol-pyruvoylshikimate-3-phosphate (EPSP) synthase as a possible target, since a strong structural similarity exists between aminomethylenebisphosphonic acid and an inhibitor of EPSP synthase, the herbicide glyphosate. This is, howeve…

Phenolic compounds of herbal infusions obtained from some species of the Lamiaceae family

Abstract The present investigation was to estimate the total phenolic content and composition of flavonoids and hydroxycinnamic acids in herbal infusions obtained from aerial parts of three Lamiaceae species (Dracocephalum moldavica, Ocimum americanum and Satureja hortensis). The total phenolic content of herbal infusions was determined using a spectrophotometric method, whereas the individual phenolics were assessed by high-performance liquid chromatography (HPLC). The HPLC method was developed and validated. The total phenolic content was measured by applying the Folin-Ciocalteu method with reference to gallic acid. Results were in the range from 29.39 to 65.38 mg estimated as gallic acid…

Preparation and characterization of dummy-template molecularly imprinted polymers as potential sorbents for the recognition of selected polybrominated diphenyl ethers.

The main aim of this work was to conduct the preliminary/basic research concerning the preparation process of a new dummy molecularly imprinted polymer (DMIP) materials. Developed DMIPs were proposed as a sorption material in solid-phase extraction (SPE) technique for recognition of selected low mass polybrominated diphenyl ethers (PBDEs) – PBDE-47 and PBDE-99. Four new DMIPs were synthesized employing bulky polymerization technique by application of structural analogue of low mass PBDEs - 4,4′-Dihydroxydiphenyl ether, as a dummy template. The DMIPs and corresponding non-imprinted polymers were prepared using different functional monomers: methacrylic acid; methyl methacrylate and different…

A useful procedure for detection of polyamines in biological samples as a potential diagnostic tool in cancer diagnosis

Abstract Background Polyamines present in human body are frequently considered as markers of occurrence of cancer. Therefore, the availability of simple and efficient method for determination of their level in body liquids and tissues is of some interest. Methods Supported liquid membrane technology coupled with HPLC seems to be an appropriate technique to follow the level of polyamines in human blood and urine. Thus, the membranes of two different geometries: flat sheet and hollow fiber were studied as a mean for separation and enrichment of studied polyamines from urine and tissue samples in order to prepare samples to be analyzed by HPLC. Conclusions Developed extraction systems offer an…

Effects of aminophosphates and their combinations with glyphosate on the growth ofLepidium sativumL. andCucumis sativusL.

Organophosphonate utilization by the wild‐type strain of cladosporium resinae

We studied the biodegradation of compounds containing phosphorus‐to‐carbon bond by using wild‐type strain of Cladosporium resinae. The substrate specificity of the strain was studied and we found that it is able to utilize a range of structurally diverse organophosphonates as a sole source of phosphorus. This ability is inducible as indicated by the presence of a lag phase of the growth. A popular herbicide glyphosate is also degraded by the fungi. This indicates that Cladosporium resinae may play an important role in biodegradation of this herbicide. The strain which we used, however, did not metabolise any phosphonates when they served as the sole carbon or nitrogen sources.

Secondary metabolites from the aerial parts of Cytisus villosus Pourr

Phytochemical investigation of the aerial parts of Cytisus villosus Pourr. resulted in the isolation and characterization of a new isoflavan, (3S, 4S)-2′,4′-dihydroxy-3′-methoxy-6,7-methylenedioxyisoflavan- 4-ol (1), and a new monoterpene, (4R,6S)-4-hydroxy-2,2,6-trimethyl-9-oxabicyclo [4.2.1] non-1(8)-en-7-one (2), together with four known flavonoids: geinstein (3), chrysin (4), chrysin -7-O-β-D-glucopyranoside (5) and 2″-O-α-L-rhamnosylorientin (6). The structures of the new compounds were elucidated on the basis of extensive spectroscopic analysis, including 1D, 2D NMR ((1)H, (13)C, COSY, TOCSY, HMBC and HSQC) and HRESIMS. The absolute configurations of 1 and 2 were established by the co…

Determination of muscimol and ibotenic acid in mushrooms of Amanitaceae by capillary electrophoresis

In this study, the CZE method for rapid quantitative and qualitative determination of ibotenic acid and muscimol in Amanita mushrooms naturally grown in Poland was developed. The investigations included the species of A. muscaria, A. pantherina, and A. citrina, collected in southern region of Poland. The studied hallucinogenic compounds were effectively extracted with a mixture of methanol and 1 mM sodium phosphate buffer at pH 3 (1:1 v/v) using ultrasound-assisted procedure. The obtained extracts were separated and determined by CZE utilizing a 25 mM sodium phosphate running buffer adjusted to pH 3 with 5% content of acetonitrile v/v. The calibration curves for both analytes were linear in…

Surfactant effect of Sb on the growth of Ag films on a sapphire substrate

It is shown that a very thin layer of Sb may be used as a surfactant to modify the growth of silver films on an insulating substrate. The conduction (percolation) current flowing through a dispersed Ag film appears at a significantly smaller thickness due to the change in the growth mode of silver islands. Some practical applications are indicated.

Polyphenols and Pharmacological Screening of a Monarda fistulosa L. dry Extract Based on a Hydrodistilled Residue By-Product

This study aimed to determine the composition and content of polyphenols in the dry extract obtained from the hydrodistilled residue by-product of the wild bergamot (Monarda fistulosa L., Lamiaceae Martinov family) herb (MFDE) and to evaluate its safety and pharmacological properties. The total phenolic content (TPC) in the MFDE was 120.64 mg GAE/g. The high-performance liquid chromatography (HPLC) analysis showed the presence of a plethora of phenolic compounds, including hydroxycinnamic acids and flavone derivatives in the MFDE, with rosmarinic acid and luteolin-7-O-glucoside being the main components. With an IC50 value of 0.285 mg/mL, it was found to be a strong DPPH radical scavenger. …

Supported liquid membrane extraction with single hollow fiber for the analysis of fluoroquinolones from environmental surface water samples

Abstract In this work, the simple analytical method for the determination of four fluoroquinolone antibiotics: ciprofloxacin, enrofloxacin, norfloxacin and danofloxacin, in environmental surface water samples is described. Sample pretreatment step was performed by the application of a technique based on supported liquid membrane extraction with the configuration of single hollow fiber (HF-SLM). The HPLC system with diode array detection was used for final analysis of studied analytes. Various parameters affecting the extraction efficiency during HF-SLM enrichment, such as type of membrane diluent, pH of donor (sample) and acceptor phases, as well as an enrichment time and salt content of sa…

Plant-growth-regulatingN-(phosphonoacetyl)amines

A series of N‐(phosphonacetyl)amine derivatives were synthesized and screened for plant‐growth regulating activity on Lepidium sativum L. and Cucumis sativus L. Aromatic N‐(phosphonoacetyl)amines. which may be considered as possible analogues of N‐acylaniline herbicides obtained by replacement of their acyl group by the phosphonacetyl moiety, exhibited significant or moderate herbicidal activity. In contrast, N‐(phosphonoacetyl)amino acids and N‐(phosphonoacetyl)aminophosphonic acids promoted the growth of L. sativum and C. sativus roots.

Herbicidal derivatives of aminomethylenebisphosphonic acid. Part III. Structure-activity relationship.

Derivatives of aminomethylenebisphosphonic acids constitute a class of promising herbicides. More than 40 N-substituted aminomethylenephosphonic acids were synthesized and evaluated for their herbicidal activity on common cress (Lepidium sativum L.) and cucumber (Cucumis sativus L.). Some of the tested compounds were found to exhibit strong herbicidal properties being equal in activity with the popular herbicide glyphosate as well as parent N-pyridylaminomethylenephosphonic acids. N-Substituted iminodi(methylenephosphonic) acids, which may be considered as close analog of glyphosate, were inactive toward test plants.

Do differences in chemical composition of stem and cap of Amanita muscaria fruiting bodies correlate with topsoil type?

Fly agaric (Amanita muscaria) was investigated using a 1H NMR-based metabolomics approach. The caps and stems were studied separately, revealing different metabolic compositions. Additionally, multivariate data analyses of the fungal basidiomata and the type of soil were performed. Compared to the stems, A. muscaria caps exhibited higher concentrations of isoleucine, leucine, valine, alanine, aspartate, asparagine, threonine, lipids (mainly free fatty acids), choline, glycerophosphocholine (GPC), acetate, adenosine, uridine, 4-aminobutyrate, 6-hydroxynicotinate, quinolinate, UDP-carbohydrate and glycerol. Conversely, they exhibited lower concentrations of formate, fumarate, trehalose, α- an…

Antifungal activity of the carrot seed oil and its major sesquiterpene compounds.

Carrot seed oil is the source of the carotane sesquiterpenes carotol, daucol and β-caryophyllene. These sesquiterpenic allelochemicals were evaluated against Alternaria alternata isolated from the surface of carrot seeds cultivar Perfekcja, a variety widely distributed in horticultural practise in Poland. Alternaria alternata is one of the most popular phytotoxic fungi infesting the carrot plant. The strongest antifungal activity was observed for the main constituent of carrot seed oil, carotol, which inhibited the radial growth of fungi by 65% at the following concentration.

Mechanical behavior and structure of single beads of homogeneous and macroporous styrene–divinylbenzene copolymers

The stress–stain and ultimate behavior in compression of homogeneous and macroporous beads of styrene–divinylbenzene copolymers has been investigated in the dry state or in equilibrium with toluene, acetone, methanol, and water. The penetration modulus A indicates sensitively the transition from the glassy into the rubbery state induced by an increase in temperature or swelling. For macroporous copolymers, A of the glassy polymers is mainly determined by the porosity P, while in the rubbery region it primarily depends on the matrix structure (degree of crosslinking and concentration and composition of the diluent). The high value of the slope s of the A vs. P dependence (s ∼ −3) for macropo…

Analytical procedure elaboration of total flavonoid content determination and antimicrobial activity of bee bread extracts

Sixteen ethanolic extracts were obtained from seven different bee bread samples. The total flavonoid content in the extracts was determined by aluminium-chloride method and was in the range of 8.3 mg/L ± 6.24% to 195.3 mg/L ± 1.35% and 28.8 mg/L ± 19.33% to 603.3 mg/L ± 4.64% with reference to quercetin and rutin, respectively. The relative standard deviations (RSD) for parallel measurements for the calibration curves of quercetin dehydrate and rutin trihydrate were in the range of 0.51% to 9.39% and 5.02% to 19.91%, respectively. The RSD for parallel measurements for the extracts with reference to quercetin dihydrate and rutin trihydrate were in the range of 0.23% to 11.64% and 4.64% to 19…

Separation of aminoalkanephosphonic acid enantiomers by indirect UV detection capillary electrophoresis with application of cyclodextrins.

Indirect UV detection capillary electrophoresis (CE) was used for the separation of aminoalkanephosphonic acid (AP) enantiomers by applying commercially available cyclodextrins as chiral discriminators. The results show that the separation of the enantiomers depends on pH of the background electrolyte, the molar ratio of cyclodextrin to aminophosphonic acid, and on the type of the applied chiral selector. Optimization of process conditions allowed enantiomeric baseline separation or partial separation of 12 out of 14 alpha-aminophosphonic acids studied. This type of CE might therefore be successfully used for routine determination of enantiomeric purity of aminophosphonic acids.

Algae and Their Extracts in Medical Treatment

Scientific efforts undertaken in recent decades have undoubtedly proven that algae are an inestimable and, what is more, important renewable source of hundreds of chemical compounds characterized by a wide spectrum of biological activity. Polysaccharides, phenolic compounds and their derivatives, pigments, proteins, lipids, and fatty acids are the substances that can be isolated from seaweeds, possessing antimicrobial, antiviral, antifungal, antilipidemic, antitumor, antidiabetic, anticoagulant, antioxidant, and antiallergic properties, which can be successfully utilized for human needs. The majority of attention has been focused on marine polysaccharides and their application in medicine a…

Determination of optical purity of phosphonic acid analogues of aromatic amino acids by capillary electrophoresis with alpha-cyclodextrin.

A simple and efficient method for the determination of enantiomeric purity of structurally diverse phosphonic and phosphinic acid analogues of phenylalanine and phenylglycine using capillary electrophoresis is presented. These preliminary studies indicated that the enantiomer separation is strongly dependent on the structure of the aminophosphonic acid.

Concentration of amino acids using supported liquid membranes with di-2-ethylhexyl phosphoric acid as a carrier

Abstract Basic studies of a procedure for extraction of amino acids using a supported liquid membrane containing di-2-ethylhexyl phosphoric acid are presented. The extractions are made from an aqueous donor phase with pH 3 to a more acidic acceptor phase and the mass transfer is driven by the proton gradient between these phases. For 0.01 mM tryptophan and with 1 M HCl as acceptor phase, an extraction efficiency of 60% is obtained, constant up to at least 12 h. This permits concentration enrichment factors linearly increasing with time up to values of at least 150. For higher amino acid concentrations, the extraction efficiency is constant only over shorter time intervals.

Inhomogeneity of gel and microsyneresis in porous styrene‐divinylbenzene copolymers

The porosity of styrene-divinylbenzene copolymers prepared by suspension copolymerisation of the monomers carried out in the presence of inert diluent changes due to solvent pretreatment is investigated. The changes seem to reflect the inhomogeneity of copolymer gel. Various portions of it are transferred from the rubber-like into the glassy state at different stages of either swelling solvent exchange or the drying process. A microsyneresis, i.e. a local collapse of loosely crosslinked gel portions not followed by a shrinkage of the whole system, leads to the porosity changes.

Chemical transformations of glucose in solutions for peritoneal dialysis after sterilization and during storage

The objective of this work was to estimate glucose degradation products (GDPs) in solutions for peritoneal dialysis (PD) including glucose and sodium lactate based on the change of pH and absorption of ultraviolet (UV) light. Spectrophotometric and pH-metric methods were used to measure glucose degradation and transformation of GDPs in laboratory-made solutions after heat sterilization and during storage. Mechanism of transformations of GDPs in the sterilized solutions for PD during storage and spectral characteristic of 5-HMF were studied. Common features for all the batches of the tested solutions for PD after heat sterilization were a reduce in pH, increase in the absorbance in the range…

Phytochemical Evaluation of Tinctures and Essential Oil Obtained from Satureja montana Herb

Winter Savory (Satureja montana L.) has been used in traditional medicine and as a spice or natural food preservative in the Mediterranean region for centuries. In this paper, some technological and analytical aspects of the S. montana tinctures development and an evaluation of the essential oil composition are provided. The total phenolic and flavonoid contents and phenolic compounds profile analyzed spectrophotometrically and by high-performance thin-layer chromatography (HPTLC), respectively, were evaluated in the developed tinctures. The results showed that the tinctures prepared from the S. montana herb by maceration or remaceration are rich in polyphenols, and there is an influence of…

Crotonic acid as a bioactive factor in carrot seeds (Daucus carota L.)

Water extracts from the carrot seed (Daucus carota L.) var. Perfekcja exhibit plant growth inhibitory properties against cress, cucumber, onion and carrot in a dose-dependant manner. This property results from the action of low-and high-molecular components of the extract. The low-molecular component was identified as crotonic acid ((E)-2-butenoic acid). Its presence was also confirmed in other late varieties of carrot. The determined strong herbicidal properties of crotonic acid and its availability after release to soil combined with its high level in seeds suggest that it might be considered as an allelopathic and autotoxic factor in the seeds.

Herbicidal activity of phosphonic and phosphinic acid analogues of glutamic and aspartic acids

Phosphonic and phosphinic acid analogues of glutamic and aspartic acids were synthesized and screened for herbicidal activity on Lepidium sativum L. Depending on the chemical structure, they exhibited significant or moderate herbicidal activity against L. sativum roots (with some representatives being equipotent with phosphinothricin), while their influence on shoot growth was negligible. Cucumis sativus L. appeared to be more tolerant to these analogues. The origin of this selectivity remains to be determined.

High-performance liquid chromatographic enantiomer separation and determination of absolute configurations of phosphinic acid analogues of dipeptides and their α-aminophosphinic acid precursors

The enantiomers of N-benzyloxycarbonyl-phosphinic pseudodipeptides and their N-benzyloxycarbonyl-α-aminophosphinic acid precursors as well as various other structural analogues were separated on a set of cinchona alkaloid-derived chiral anion-exchangers by HPLC in the reversed-phase mode. Semi-preparative scale chromatography provided single enantiomers in 100 mg quantities. The configurations of the enantiomers were assigned indirectly by enantioselective chromatography on the basis of the elution order and was confirmed by enantiomeric reference compounds.

Herbicidally Active Derivatives of Aminomethylenebis-Phosphonic Acid-Mode of Action and Structure - Activity Relationship

Abstract: (N-pyridylamino)methylenebisphosphonates exhibit strong herbicidal activity which may be reversed by supplementation of the growth media with aromatic amino acids. They appeare to be the inhibitors of aromatic amino acids biosynthesis acting as inhibitors of DAHP synthase the first enzyme of shikimate pathway. Over 40 analogues of these acids were synthesized in order to determine the structure-activity relationship.

Extraction of dansylated amino acids using the supported liquid membrane technique

Extraction using the supported liquid membrane (SLM) technique demands conditions where the extracted compounds can be made uncharged allowing them to pass through the membrane. For amino acids, being bifunctional, such conditions can not be obtained directly. One way to overcome this problem is to block one of the functionalities by derivatization, utilising the other group for the transport. The SLM extraction of dansylated amino acids was investigated and optimized. It was possible to obtain high extraction efficiencies (>90%) for most amino acids. For amino acids with polar side chains, such high extraction efficiencies were only obtained at low analyte concentrations ( 10 nmol 1-l). Fo…

Enantioselective transport of amino acid through supported chiral liquid membranes

Abstract Two chiral alcohols, nopol and (2S)-(−)-methyl-1-butanol, immobilized in the pores of a polyethylene film were used for the anantioselective transport of amino acid hydrochloride. The degree of stereoselectivity of the permeation process varied from 0.39 to 1.52 depending on both the type of the chiral membrane phase and the properties of the amino acid. The evaluation of the membrane ability to separate stereoisomers was performed by the step-by-step analysis by considering the effect of amino acids' hydrophobicity, polarity and degree of chirality. For the purpose of this paper, the chirality measure was introduced. It was demonstrated that the enantioselectivity was affected mai…

Presence of plant hormones in composts made from organic fraction of municipal solid waste

Composting is a process of the biological decomposition of organic matter under aerobic conditions. Composts made from waste may still contain other substances that influence plant growth and development, such as vitamins or plant growth substances (plant hormones). Application of products containing phytohormones has an effect on numerous physiological processes in plants. Among observable results are: improved condition of the root system, increased absorption of nutrients, improved stress and disease resistance and delayed aging. The purpose of the research was to analyse the occurrence of plant hormones in mature composts made from selectively collected organic fraction of household mun…

Application of molecularly imprinted polymers in analytical chiral separations and analysis

Over the last two decades the process of development and application of a new types of molecular imprinted polymer (MIP) sorbents in the field of analytical chemistry have been widely described in the literature. One of the new trends in analytical chemistry practice is the use of new types of MIP sorbents as specific sorption materials constituting the stationary phase in advanced separation techniques. The following review paper contains comprehensive information about the application of a specific and well defined MIP sorbents (with the data base in the paper about the reagents used in MIP preparation process) as stationary phases in separation techniques including high performance liqui…

Research on Acute Toxicity and the Behavioral Effects of Methanolic Extract from Psilocybin Mushrooms and Psilocin in Mice

The pharmacological activities and acute toxicity of the psilocin (PC) and dried residues of the crude extracts of psychotropic mushrooms were investigated in mice. The hallucinogenic substances were effectively isolated, by using methanol, from the species of Psilocybe semilanceata and Pholiotina cyanopus, that were collected in the north-east region of Poland. The chemical analysis of these extracts, which was performed by liquid chromatography with mass spectrometry detection (LC-MS), indicated the presence of psilocin and other hallucinogenic substances, including indolealkylamines and their phosphorylated analogues. When the pure psilocin or fungal extracts were used, slight difference…

Valuable natural products from marine and freshwater macroalgae obtained from supercritical fluid extracts

The biologically active compounds (fatty acids, pigments, phenolics, and flavonoid content) were studied in supercritical fluid extracts from the biomass of marine (Ulva clathrata, Cladophora glomerata, Polysiphonia fucoides, and their multi-species mixture) and freshwater (C. glomerata) macroalgae. Different extraction techniques were used in order to compare differences in the biologically active compound composition of the macroalgal extracts. The results indicated that the saturated and unsaturated fatty acids ranged from C9:0 to C22:0. The analysis of differences in the composition of unsaturated to saturated fatty acids in extracts showed that palmitic acid (C16:0) and oleic acid (C18…

Supported Liquid Membranes and Their Modifications

Publisher Summary This chapter discusses the principle, kinetic and transport mechanisms, stability of supported liquid membrane (SLM) design followed by thier configuration. In the examples of SLM applications presented in this chapter, the possibility to separate high quantities of compounds using small volumes of organic phases shows that this method is still a very attractive choice when an efficient and selective method is necessary. Also, as a result of the development and commercialization of hydrophobic hollow-fiber membrane contactors, SLM might be applied successfully for industrial purposes. This is due to the high-membrane surface per unit of volume with satisfactory liquid memb…

Surface molecularly imprinted silica for selective solid-phase extraction of biochanin A, daidzein and genistein from urine samples

Selective molecularly imprinted silica polymer (SiO2MIP) for extraction of biochanin A, daidzein and genistein was synthesized using the surface molecular imprinting technique with the silica gel as a support. Biochanin A (BCA) was used as a template, 3-aminopropyltriethoxysilane (APTES) as a functional monomer, and tetraethoxysilicane (TEOS) as a cross-linker. Non-imprinted polymer with the sol–gel process (SiO2NIP) was also prepared for comparison. The synthesized polymers were characterized by Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM) and a standard Brunauer-Emett-Teller (BET) and Barret–Joyner–Halenda (BJH) analysis. The obtained results indicate…

Immuno-SLM—a combined sample handling and analytical technique

Immuno-supported liquid membrane (immuno-SLM) extraction is a new technique that makes use of antibody (Ab)-antigen interactions as the "extraction force" to drive the mass transfer in a selective way. In immuno-SLM, anti-analyte (Ag) Abs are introduced into the acceptor phase of the SLM unit to trap the Ag that passes from the flowing donor through the SLM into the stagnant acceptor. The amount of immuno-extracted analyte (AbAg) is quantified by connecting the immuno-SLM unit on-line with a non-competitive heterogeneous fluorescence flow immunoassay (FFIA) that makes use of a fluorescein-labeled analyte tracer that titrates the residual excess of Ab present in the acceptor. A restricted ac…

Effect of extraction solvent on total phenolic content, total flavonoid content and antioxidant activity of Cetraria islandica

Oxidative stress may lead to a number of diseases such as atherosclerosis, nephrotoxicity, liver cirrhosis, cancers, diabetes, and Alzheimer disease. Medicinal plants are an important source of antioxidants. Therefore, the antioxidant potential of Cetraria islandica was evaluated in this work. The coarse powder of leaf of Cetraria islandica was extracted in Soxhlet apparatus, with ethanol (90%) and ethanolic extract of Cetraria islandica (EECI) was further processed for phytochemical screening, total phenol content, total flavonoid content, and various in vitro antioxidant assays. The phytochemicals present in EECI were glycosides, carbohydrates, triterpenoids, proteins and amino acids, gum…

Separation of aromatic aminophosphonic acid enantiomers by capillary electrophoresis with the application of cyclodextrins

The detailed studies concerning capillary electrophoresis separation of aminophosphonic acid enantiomers with various commercially available cyclodextrins are presented. The obtained results show that the separation of these stereoisomers is dependent on pH of background electrolyte, concentration of cyclodextrin as well as on the type of applied chiral selector. The separation mechanism is based on the co-operative effect of hydrogen bond type interactions enhanced by hydrophobic forces and sterical constrains between aminophosphonate and cyclodextrin. With application of elaborated method, enantiomeric baseline or partial separation of 18 alpha-aminophosphonic acids was achieved. This sep…

Herbicidal activity of phosphonic, phosphinic, and phosphonous acid analogues of phenylglycine and phenylalanine

A series of phosphonic, phosphinic, and phosphonous acid analogues of phenylglycine and phenylalanine was synthesized and tested as herbicides against Lepidium sativum and Cucumis sativus. Aminobenzylphosphonic acids exhibited notable herbicidal activity and thus represent a group of the most active herbicides found among aminophosphonic acids.

Biologically Active Organic Compounds, Especially Plant Promoters, in Algae Extracts and Their Potential Application in Plant Cultivation

Enantiomeric separation of amino acids by capillary electrophoresis with α-cyclodextrin

A simple method for separation of underivatized aromatic amino acid enantiomers is presented. The influence of α-cyclodextrin concentration, applied voltage and background buffer pH on the separation were investigated to achieve the best conditions of separation.

Application potential of dummy molecularly imprinted polymers as solid-phase extraction sorbents for determination of low-mass polybrominated diphenyl ethers in soil and sediment samples

Abstract Despite the introduction of restrictive regulations in the USA and the European Union, polybrominated diphenyl ethers (PBDEs) are still found in various types of environmental and biological samples at significant concentration levels. The presence of these persistent organic pollutants in the environment raises important issues because of their negative impact on immunological and neurological systems, and on the hormonal balances in living organisms. From the analytical point of view, the final determination of PBDEs would entail substantial challenges, because it would necessitate conducting the pre-concentration of analytes, or sample clean up. The aim of the present study is t…

Sample pretreatment techniques for oligopeptide analysis from natural sources

The analysis of oligopeptides in samples of food, tissues, and body fluids attracts considerable attention. The complexity of such samples requires efficient sample preparation (i.e., concentration and cleanup) procedures to remove interfering endogenous compounds and inorganic or organic salts. The methods of sample pretreatment that enable effective and selective isolation and/or preconcentration of oligopeptides from complex sample matrices have been reviewed. In each case, examples of application were presented and discussed, taking into account selectivity, enrichment, method automation, cleanup, and environmental aspects of the developed methods.

Facilitated SLM extraction of peptides with D2EHPA as a carrier

Abstract The extraction of short peptides through a supported liquid membrane containing di-2-(ethylhexyl)phosphoric acid (D2EHPA) as a carrier was investigated. The extraction was carried out from the aqueous donor phase with pH 3 to amore acidic acceptor phase. The proton gradient between the donor and the acceptor phase was the main driving force of the mass transfer in this system. The influence of various parameters such as diluent of the carrier, pH of the donor and acceptor phase, peptide structure and concentration on the extraction efficiency was presented.

Applications of Electromigration Techniques: Applications of Electromigration Techniques in Food Analysis

Electromigration techniques, including capillary electrophoresis (CE), are widely used for separation and identification of compounds present in food products. These techniques may also be considered as alternate and complementary with respect to commonly used analytical techniques, such as high-performance liquid chromatography (HPLC), or gas chromatography (GC). Applications of CE concern the determination of high-molecular compounds, like polyphenols, including flavonoids, pigments, vitamins, food additives (preservatives, antioxidants, sweeteners, artificial pigments) are presented. Also, the method developed for the determination of proteins and peptides composed of amino acids, which …

Using Macroelement Content to Characterize Surficial Water Quality of Artificial Reservoirs

Abstract The quality of surface waters in the territory of Poland, despite the implemented remedial measures, is mostly classified as bad. This article presents the results of research on the composition of water macroelements in 24 artificial reservoirs located in Opole province (southern Poland), searching for the reasons behind their pollution. Concentrations of the anions F−, Cl−, Br−, NO2−, NO3−, PO43− and SO42− and cations Na+, NH4+, K+, Mg2+ and Ca2+ were taken into account. An analysis of seasonal changes was carried out and, on the example of a dam reservoir (Turawa Big Reservoir), a multi-point analysis of the distribution of ion concentrations in water at the reservoir surface w…

Transport of dipeptides and phosphono dipeptides through an immobilized liquid membrane. Stereoselectivity of the process

Abstract Dipeptide and phosphono dipeptide hydrochlorides permeated well through a 1-decanol membrane supported in a porous polyethylene hollow fiber matrix. This transfer is easily accomplished either by passive or by carrier-facilitated (with Kryptofixes 222 or 5 present in the membrane phase) transport. The transport is stereoselective with l-l dipeptides being transported faster than their l-d isomers.

Extraction of short peptides using supported liquid membranes

Studies of extraction of short peptides using supported liquid membranes containing Aliquat 336 as a carrier are presented. The extractions are carried out from an aqueous donor phase with pH ≥ 10 to an acceptor phase containing salt. The mass transfer is driven by the gradient of salt concentration between these phases. The extraction efficiency is dependent on the composition of water phases, the type and concentration of counter-ion in the stagnant acceptor phase and the flow rate of the donor phase. Moreover, it is also influenced by the concentration and structure of the examined peptides.

Bioactive Alkaloids of Hallucinogenic Mushrooms

Abstract The aim of our chapter is to review recent developments in a group of medicinally important natural products–alkaloids, with reference to the structure–activity studies in respect of certain diseases. Alkaloids covered by our review come from mushrooms called “hallucinogenic.” Hallucinogenic compounds have been chemically identified in mushrooms belonging to various genera, e.g., Agrocybe, Amanita, Conocybe, Galerina, Gymnopilus, Hypholoma, Inocybe, Panaeolus, Psilocybe, Pholiotina, Pluteus, and Weraroa [J.W. Allen, Ethnomycol. J. Sacred Mushroom Stud. 9 (2012) 130–175]. One of the largest classes of alkaloids is indole alkaloids. Indoles are probably the most widely distributed he…

Multivariate optimization of the hollow fibre liquid phase microextraction of muscimol in human urine samples.

Abstract A liquid phase microextraction based on hollow fibre followed by liquid chromatographic determination was developed for the extraction and quantitation of the hallucinogenic muscimol from urine samples. Method applicability on polar hallucinogens was also tested on two alkaloids, a psychedelic hallucinogen, tryptamine and a polar amino acid, tryptophan which exists in its charged state in the entire pH range. A multivariate design of experiments was used in which a half fractional factorial approach was applied to screen six factors (donor phase pH, acceptor phase HCl concentration, carrier composition, stirring rate, extraction time and salt content) for their extent of vitality i…