A procedure for arsenic species fractionation in alga samples (Sargassum fulvellum, Chlorella vulgaris, Hizikia fusiformis and Laminaria digitata) by extraction is described. Several parameters were tested in order to evaluate the extraction efficiency of the process: extraction medium, nature and concentration (tris(hydroxymethyl)aminomethane, phosphoric acid, deionised water and water/methanol mixtures), extraction time and physical treatment (magnetic stirring, ultrasonic bath and ultrasonic focussed probe). The extraction yield of arsenic under the different conditions was evaluated by determining the total arsenic content in the extracts by ICP-AES. Arsenic compounds were extracted in 5 mL of water by focussed sonication for 30 s and subsequent centrifugation at 14,000 × g for 10 min. The process was repeated three times. Extraction studies show that soluble arsenic compounds account for about 65% of total arsenic.
An ultrafiltration process was used as a clean-up method for chromatographic analysis, and also allowed us to determine the extracted arsenic fraction with a molecular weight lower than 10 kDa, which accounts for about 100% for all samples analysed.
Speciation studies were carried out by HPLC–ICP-AES. Arsenic species were separated on a Hamilton PRP-X100 column with 17 mM phosphate buffer at pH 5.5 and 1.0 mL min−1 flow rate. The chromatographic method allowed us to separate the species As(III), As(V), MMA and DMA in less than 13 min, with detection limits of about 20 ng of arsenic per species, for a sample injection volume of 100 μL. The chromatographic analysis allowed us to identify As(V) in Hizikia (46 ± 2 μg g−1), Sargassum (38 ± 2 μg g−1) and Chlorella (9 ± 1 μg g−1) samples. The species DMA was also found in Chlorella alga (13 ± 1 μg g−1). However, in Laminaria alga only an unknown arsenic species was detected, which eluted in the dead volume. 相似文献
Abstract The adsorption process of four metals in solution (Pb, Cu, Zn, Cd) to Chlorella Vulgaris will be described and compared to a previous study using three metals (Pb,Cu,Zn) in solution. The binding capacity of Chlorella Vulgaris to four elements simultaneously increases with time, mass of algae, and up to a temperature of about 20.0°C. The equilibrium points for binding three metals simultaneously are at pH=4.55, with 7 mg of algae, and after 2.0 hrs. in a 5 ml aliquot of the solution. In the four metal system, the optimum values are significantly higher while the binding capacity is reduced. The competition between metals for binding sites in the algal cells is governed by kinetic properties as related to the pH, mass of algae, time, and concentration of solution. The binding process is also dependent upon thermodynamics with respect to the temperature of the solution. 相似文献
Chitosan resins, which clinically served as adsorbents in hemo perfusion therapy, were prepared with reversed-phase suspension
methodology using three differently structured crosslinking agents, methanal, glyoxal and glutaraldehyde. And the glyoxal
and glutaraldehyde crosslinked chitosan resins were reduced with NaBH4 afterwards. By analyzing the results from FTIR and SEM, it was found that the reduction treatment to the adsorbents efficiently
improved the chemical stability of these chitosan resins, and the shifts in crosslinking agents exerted influences over the
morphologies of the adsorbents obviously. After being put to use in the adsorption tests upon some model uremic middle molecular
toxins and BSA in vitro, all three adsorbents demonstrated a fairly realistic adsorption capability to the model toxins but
little to BSA. And the adsorption process reached the equilibrium in a clinically qualified short time. But the adsorption
capacities of these adsorbents to the model toxins were quite different. It had been found that with the growing of fatty
chain length of crosslinking agent, these adsorbents showed a gradually increased adsorption capacity to the model toxins,
and the glutaraldehyde crosslinked chitosan resin behaved best. 相似文献
AbstractThe application of algae to the most meaningful fields of our life, such as food, environment and energy, finds a further confirmation in the extension of this application to cultural heritage protection. In this letter, we present the results of a preliminary study testing how a polysaccharide extracted from algal matrix can restore degraded paper giving back it mechanical strength and chemical structure. 相似文献
Recent methods employed for the analysis of algal toxins have focused on high performance liquid chromatography. However these methods suffer from poor resolution, poor efficiency, and long analysis times. This study involves the investigation of a number of toxins including nodularin, microcystin LR, YR, and RR which are cyclic peptides produced by strains of blue-green algae. The electroseparation mode was micellar electrokinetic capillary chromatography (MECC) using a borate buffer containing sodium dodecyl sulfate (SDS) as the surgactant of choice. The method was optimized with standard toxin compounds and employed for the screening opf toxins in supercritical fluid extracts (SFE) of freeze-thawed algal scum samples. 相似文献
The human toxic syndrome, diarrhetic shellfish poisoning (DSP), is caused by polyether toxins that are present in bivalve molluscs but originate from some species of marine phytoplankton. During the last few years different HPLC methods with fluorescence detection (FLD) have been proposed for analysis of marine toxins, including polyether toxins, in shellfish and phytoplankton. Several derivatization reagents have been proposed in the literature, with the aim of converting the acidic DSP toxins into their corresponding fluorescent derivatives. In this work we report results obtained from HPLC–FLD analysis of extracts from phytoplankton, including Dinophysis spp., harvested off the south-west coast of Ireland. Three different reagents were used for fluorescent derivatization: 3-bromomethyl-6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone (BrDMEQ), 9-chloromethylanthracene (CA), and in situ 9-anthracenyldiazomethane (ADAM). Derivatization was performed under conditions previously optimised. The DSP derivatives were cleaned using different SPE procedures then analysed by HPLC–FLD. In this study, the use of BrDMEQ, CA, and in situ ADAM was compared in terms of sensitivity and selectivity. Evaluation of HPLC methods for analysis of DSP toxin derivatives was also conducted; the presence of okadaic acid (OA), dinophysistoxin-2 (DTX-2), and pectenotoxin-2 seco acids (PTX1SAs) was detected in the sample extracts studied. 相似文献
Hydrophilic interaction liquid chromatography (HILIC) was examined for the separation of paralytic shellfish poisoning (PSP) toxins using the stationary phase TSK-gel Amide-80. The parameters tested included type of organic modifier and percentage in the mobile phase, buffer concentration, pH, flow rate and column temperature. Using mass spectrometric (MS) detection, the HILIC column allowed the determination of all the major PSP toxins in one 30 min analysis with a high degree of selectivity and sensitivity. The high percentage of organic modifier in the mobile phase and the omission of ion pairing reagents, both favored in HILIC, provided limits of detection (LOD) in the range 50-100 nM in selected ion monitoring (SIM) mode on a single quadrupole LC-MS system. LOD in selected reaction monitoring (SRM) mode on a sensitive triple quadrupole system were as low as 5-30 nM. Excellent linearity of response was observed. 相似文献