Speciation analysis of antimony in marine biota is not well documented, and no specific extraction procedure of antimony species from algae and mollusk samples can be found in the literature. This work presents a suitable methodology for the speciation of antimony in marine biota (algae and mollusk samples). The extraction efficiency of total antimony and the stability of Sb(III), Sb(V) and trimethylantimony(V) in different extraction media (water at 25 and 90 °C, methanol, EDTA and citric acid) were evaluated by analyzing the algae Macrosystis integrifolia (0.55 ± 0.04 μg Sb g−1) and the mollusk Mytilus edulis (0.23 ± 0.01 μg Sb g−1). The speciation analysis was performed by anion exchange liquid chromatography (post-column photo-oxidation) and hydride generation atomic fluorescence spectrometry as detection system (HPLC-(UV)-HG-AFS). Results demonstrated that, based on the extraction yield and the stability, EDTA proved to be the best extracting solution for the speciation analysis of antimony in these matrices. The selected procedure was applied to antimony speciation in different algae samples collected from the Chilean coast. Only the inorganic Sb(V) and Sb(III) species were detected in the extracts. In all analyzed algae the sum of total antimony extracted (determined in the extracts after digestion) and the antimony present in the residue was in good agreement with the total antimony concentration determined by HG-AFS. However, in some extracts the sum of antimony species detected was lower than the total extracted, revealing the presence of unknown antimony species, possibly retained on the column or not detected by HPLC-(UV)-HG-AFS. Further work must be carried out to elucidate the identity of these unknown species of antimony. 相似文献
More discerning than the parent : Analogues of the polyamine toxin argiotoxin 636 (shown docked in the ion channel of an ionotropic glutamate (iGlu) receptor; N blue, O red) distinguish subtypes of iGlu receptors. Depending on which of the two internal amine groups is replaced with a methylene group, the analogue inhibits one or other of two receptor subtypes as potently as the natural compound, which itself inhibits both subtypes nonselectively.
An efficient and versatile synthesis of acylpolyamine spider toxins of all structural types classified by extensive MS analysis has been achieved. By using 2-nitrobenzenesulfonamide as an effective activating and/or protecting group (the Nosyl strategy), the naturally occurring toxins 1-8 corresponding to Types A-F were concisely synthesized in high overall yield. 相似文献
Collision-induced dissociation (CID) mass spectra were generated for azaspiracids using electrospray ionisation (ESI), and hydrogen/deuterium (H/D) exchange was used to ascertain the number and type of replaceable hydrogens in the three predominant azaspiracid toxins. H/D exchange was conveniently achieved using deuterated solvents for liquid chromatography (LC). Using ion-trap mass spectrometry, multiple-stage CID experiments (MS(n)) on the protonated and fully exchanged ions were performed to decipher characteristic fragmentation pathways. The precursor and product ions from azaspiracids lost up to five water molecules from different regions during MS(n) experiments and it was possible to distinguish between the water losses from different molecular regions. These studies confirmed that the first water-loss ion in the spectra of azaspiracids resulted from dehydration at the vicinal diol at C20-C21. Five MS dissociation pathways were identified that resulted from fragmentation of the carbon skeleton of azaspiracids producing nitrogen-containing ions. Two pathways, involving cleavage of the E-ring and C27-C28, gave ions that were found in all azaspiracids. Three pathways, A-ring, C-ring and C19-C20 cleavages, were useful for distinguishing between azaspiracid analogues. The same product ions from backbone fragmentation were also observed using hybrid quadrupole time-of-flight mass spectrometry (QqTOFMS). The fragmentation of the A-ring was the most facile and was exploited in the development of LC/MS(n) methods for the analysis of azaspiracids. 相似文献
The synthesis of different protected alternariol derivatives using intramolecular cyclization of iodoresorcylic acid phenyl esters by palladium-catalyzed C–H activation as key step is presented. Furthermore, chemical sulfation and glucosylation were applied for the preparation of conjugated Alternaria mycotoxins. These compounds are suspected to be formed during metabolism in contaminated plants. Therefore, all synthetic conjugates prepared within this work serve as reference materials for further studies in the fields of bioanalytics and toxicology of mycotoxins. 相似文献
Freshwater and brackish microalgal toxins, such as microcystins, cylindrospermopsins, paralytic toxins, anatoxins or other neurotoxins are produced during the overgrowth of certain phytoplankton and benthic cyanobacteria, which includes either prokaryotic or eukaryotic microalgae. Although, further studies are necessary to define the biological role of these toxins, at least some of them are known to be poisonous to humans and wildlife due to their occurrence in these aquatic systems. The World Health Organization (WHO) has established as provisional recommended limit 1 μg of microcystin-LR per liter of drinking water. In this work we present a microsphere-based multi-detection method for five classes of freshwater and brackish toxins: microcystin-LR (MC-LR), cylindrospermopsin (CYN), anatoxin-a (ANA-a), saxitoxin (STX) and domoic acid (DA). Five inhibition assays were developed using different binding proteins and microsphere classes coupled to a flow-cytometry Luminex system. Then, assays were combined in one method for the simultaneous detection of the toxins. The IC50's using this method were 1.9 ± 0.1 μg L−1 MC-LR, 1.3 ± 0.1 μg L−1 CYN, 61 ± 4 μg L−1 ANA-a, 5.4 ± 0.4 μg L−1 STX and 4.9 ± 0.9 μg L−1 DA. Lyophilized cyanobacterial culture samples were extracted using a simple procedure and analyzed by the Luminex method and by UPLC–IT-TOF-MS. Similar quantification was obtained by both methods for all toxins except for ANA-a, whereby the estimated content was lower when using UPLC–IT-TOF-MS. Therefore, this newly developed multiplexed detection method provides a rapid, simple, semi-quantitative screening tool for the simultaneous detection of five environmentally important freshwater and brackish toxins, in buffer and cyanobacterial extracts. 相似文献
The use of brewery residues—yeast and trub—has been evaluated aiming to minimize the costs of the industrial production of
Bacillus sphaericus-based bioinsecticide. Both brewery residues promoted growth and sporulation of the three B. sphaericus strains that were isolated from Brazilian soils (S1, S2, and S20). However, distinct growth and sporulation behaviors were
observed in relation to the different nutritional conditions and strain used. The maximum sporulation percentage was obtained
through the cultivation of S20 strain in brewery residual yeast. In general, the entomopathogenic biomasses produced showed
good results for toxicity to Culex larvae. The minimum values of larvae population (LC50) were observed for the S20 strain grown on yeast brewery residue-containing
media. After fermentation, a considerable decrease in the organic material of alternative media was verified, although the
residual values were still higher than that considered appropriate for effluent discharge. 相似文献
Attraction and repulsion are responses to chemical stimuli which can be received and processed even by unicellular organisms without a morphologically defined nervous system. Chemical substances trigger off a chain of events which starts with a membrane-bound signal receptor and, after a sequence of regulatory and modulatory steps, ends in the modulation of a motor effector organ. Binding of the signal substances to the receptor produces conformational changes in which the receptor subunits are mutually dependent on one another, and also leads to chemical modification of the subunits and affects their molecular activity. These interactions, together with the characteristic type of movement, result in a physiological pattern of behavior which enables the flagellated sex cells (gametes) of marine brown algae to finally locate their partners. The simple but highly specific brown algae gamete systems have been investigated structurally and their biological activity analyzed. The signal substances are mainly highly unsaturated aliphatic or cyclic hydrocarbons with unsaturated side chains (general formula e. g. C11H14, C11H16, C11H18). These systems also serve as a simplifying model which helps in the understanding of complex ganglionic pathways in higher living organisms where the sense organs convey information from the surroundings to the central nervous system through nerve pathways. The information is then processed and answered, via efferent pathways, as movement. 相似文献