PubMed Health⌕ Search

Biomedical subjects

C Cámara

Publications and source records attributed to C Cámara.

32 records · Page 2Linked to original sources

Trace-level determination of triazines and several degradation products in environmental waters by disk solid-phase extraction and micellar electrokinetic chromatography.

An analytical method combining disk solid-phase extraction with micellar electrokinetic chromatography has been developed for the determination of atrazine, simazine, hydroxyatrazine, deisopropylatrazine, deethylatrazine, propazine and prometryn in water samples. The influence of the buffer and sodium dodecyl sulfate (SDS) concentration, pH and organic modifier on the separation has been studied. Baseline separation of the seven triazines was achieved under the following conditions: 10 mM borate buffer, 60 mM SDS, 20% methanol and pH 9.2. C18-bonded silica and poly(styrene-divinylbenzene) (PS-DVB) disks were evaluated for solid-phase extraction of the selected pesticides (11 of water sample). Using two PS-DVB disks, quantitative recoveries were obtained for all pesticides tested. The method was successfully applied for the determination of the seven triazines in drinking and well water at the 0.1 microg l(-1) and 0.5 microg l(-1) concentration levels, respectively. The detection limits for these analytes using the proposed analytical method were within the 0.02-0.06 microg l(-1) range in drinking water and the 0.06-0.30 microg l(-1) range in well water.

Buffers↗

Expression of high amounts of the CD117 molecule in a case of B-cell non-Hodgkin's lymphoma carrying the t(14:18) translocation.

The c-kit proto-oncogen (CD117) has been described to be present in normal and neoplastic hemopoietic cells including both myeloid and lymphoid lineages. Among the normal lymphoid cells CD117 expression would be restricted to a small subset of NK-cells, and to early T-cell precursors and it is not expressed by normal B-cells. Regarding chronic lymphoproliferative disorders the only data provided up to now suggests that CD117 expression is restricted to cases of Hodgkin's disease and anaplastic large-cell lymphoma. In the present paper we describe a case of a B-cell chronic lymphoproliferative disorder carrying the t(14:18) translocation as demonstrated by molecular studies, in which the flow cytometric immunophenotypic analysis of both peripheral blood and bone marrow samples revealed the expression of high amounts of the CD117 antigen in the surface of the clonal B-cell population. Further studies are necessary to explore both the functional role of c-kit expression in the neoplastic B-cells from this patient and its potential utility for the diagnosis and follow-up of patients with B-cell non-Hodgkin's lymphoma.

Aged↗

Selenium speciation in animal tissues after enzymatic digestion by high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry.

A procedure is described for the enzymatic digestion of tuna and mussel samples that allows the determination of selenium species by high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry. The species were extracted by two-step enzymatic hydrolysis with a non-specific protease (subtilisin). The selenium species were separated on a Spherisorb 5 ODS/AMINO column using two different chromatographic conditions, namely phosphate buffers at pH 2.8 and pH 6.0 as mobile phases. The method determines organic (trimethylselenonium, selenocystine, selenomethionine and selenoethionine) and inorganic selenium species (selenite and selenate), but only organic selenium species were found in the samples. The sum of identified selenium species in the sample was about 30% of the total selenium present in the enzymatic extract despite the fact that recoveries of total hydrolysed selenium were 93-102%. Trimethylselenonium ion and selenomethionine were found in both tuna and mussel samples and an unknown selenium species was also found in tuna samples.

Animals↗

Modification of capillaries coupled to micro-flow nebulizers: a new strategy for on-line interference removal in inductively coupled plasma mass spectrometry.

The application of interference removal within modified silica capillaries for the introduction of liquid samples by a micro-flow nebulizer into an inductively coupled plasma quadrupole mass spectrometer is described using the example of (103)Rh and its mass interferences resulting from (63)Cu (ArCu(+)), (87)Rb (RbO(+)), (87)Sr (SrO(+)) and (206)Pb (Pb(2+)). A strong cation exchanger was covalently bound to the capillary surface and its ability to interact with cations in aqueous solution was investigated. At pH 7. 0 the interfering elements can be selectively adsorbed within the capillaries without hampering the elution of Rh. The capillaries are easily regenerated by flushing with 10(-3) M hydrochloric acid in order to exchange retained cations for protons. Calibrations show no significant difference between the absence and presence of interfering elements, so the detection limit for Rh of 6.0 ng l(-1) (3sigma) is not influenced by adding up to a 100-fold excess of interferents. The method developed is compared with a mathematical correction model for inductively coupled plasma mass spectrometry using the example of Rh determination in particulate car exhaust fumes and the results obtained are discussed.

Calibration↗

Microwave-assisted extraction method for the determination of atrazine and four organophosphorus pesticides in oranges by gas chromatography (GC).

A simple and rapid microwave assisted extraction (MAE) method is presented for the determination of atrazine and four organophosphorus pesticides (parathionmethyl, chlorpyriphos, fenamiphos and methidathion) in orange peel. The experimental variables that affect the MAE method, such as temperature, sample quantity, extraction time, nature and volume of organic solvents, were optimized. The MAE method was optimized using an experimental design. The results suggest that temperature and sample quantity are statistically significant factors. It was concluded that the five pesticides could be efficiently extracted from 1.5-2.5 g of orange peel with 10 mL of hexane/acetone (1: 1) mixture at 90 degrees C in 9 min with microwave power set at 50% (475 W). After optimization these factors, recoveries ranged from 93 to 101% with a relative standard deviation ranging from 1 to 3%. The extracts were analyzed by gas chromatography with a nitrogen-phosphorus detector (GC-NPD).

Atrazine↗

Stability of inorganic mercury and methylmercury on yeast-silica gel microcolumns: field sampling capabilities.

The stability of methylmercury and inorganic mercury retained on yeast-silica gel microcolumns was established and compared with the stability of these species in solution. Yeast-silica gel columns with the retained analytes were stored for two months at three different temperatures: -20 degrees C, 4 degrees C and room temperature. At regular time intervals, both mercury species were eluted and quantified by cold vapor atomic absorption spectrometry (CVAAS). Methylmercury was found stable in the columns over the two-month period at the three different temperatures tested while the concentration of inorganic mercury decreased after one week's storage even at -20 degrees C. These results are of great interest since the use of these microcolumns allows the preconcentration and storage of mercury species until analysis, thus saving laboratory space and avoiding the problems associated with maintaining species integrity in aqueous solution.

Drug Stability↗

Feasibility study prior to the certification of trace elements in urban and industrial wastewater reference materials.

Reliable results for the determination of trace elements in urban and industrial wastewaters are of paramount importance for both checking the performance of sewage treatment and for detecting possible urban or industrial contamination sources. The quality control of measurements should in principle rely on external tools such as certified reference materials (CRM), which should represent, as closely as possible, the matrix of samples currently analysed, e.g., in the frame of environmental monitoring. To date, however, no CRM representatives of wastewater composition are available, which limits the possibility for control laboratories to check their QC externally. To fill this gap, the European Commission's Standards, Measurements and Testing Programme (formerly BCR) has started a European collaborative project of which the aim is to test the feasibility of preparation of wastewater reference materials and the analytical state-of-the-art to enable the certification of trace elements in such matrices. This paper presents the results of the first phase of this project, namely the feasibility study and the results of an interlaboratory trial.

Certification↗

Mixed immunosorbent for selective on-line trace enrichment and liquid chromatography of phenylurea herbicides in environmental waters.

An immunosorbent containing antiisoproturon and antichlortoluron antibodies immobilised on aldehyde-activated silica was employed for the on-line preconcentration and liquid chromatography-diode array detection of several phenylureas. The efficiency of the coupling of the immunosorbent to the liquid chromatographic system and the characteristics of the immunosorbent were evaluated. The on-line system allowed the selective trace enrichment of chlortoluron, isoproturon, metobromuron, linuron and chlorbromuron at the 0.05-0.5 microgram l-1 level in ground and river waters and provided detection limits in the range 0.01-0.03 microgram l-1 by percolating only 10 ml of water sample. The proposed method was validated by analysing freeze-dried tap water samples with a high content in pesticides of different chemical functionalities. The results obtained were compared with the mean value obtained in an interlaboratory exercise.

Chromatography, Liquid↗

Evaluation of high-performance liquid chromatography for the separation and determination of arsenic species by on-line high-performance liquid chromatographic-hydride generation-atomic absorption spectrometry.

An on-line high-performance liquid chromatographic-microwave assisted oxidation-hydride generation-atomic absorption spectrometric (HG-AAS) system (using columns of different kinds) has been developed for the determination of arsenite, arsenate, dimethylarsinate (DMA), monomethylarsonate (MMA), arsenobetaine (AsB) and arsenocholine (AsC) in environmental samples. Ion-pair reversed-phase chromatography using tetrabutylammonium phosphate as the ion-pair reagent and anion-exchange chromatography were evaluated and the analytical performances of each are reported. The detection limits were 97-143 and 10-30 micrograms l-1 for ion-pair reversed-phase and anion-exchange chromatography, respectively. The Hamilton PRP-X 100 anionic column was proposed for the determination of the six species; AsB can be quantitated independently of AsC by taking the difference between readings at pH 6 and pH 10.7. The proposed methods were applied to water samples and sediments and their potential for future application was demonstrated.

Arsenicals↗

Speciation of methylmercury and Hg(II) using baker's yeast biomass (Saccharomyces cerevisiae). Determination by continuous flow mercury cold vapor generation atomic absorption spectrometry.

Baker's yeast cells (Saccharomyces cerevisiae) were successfully used to selectively separate methylmercury and Hg(II). Several parameters affecting the degree of biosorption and the binding kinetics of methylmercury and Hg(II) were evaluated: solution pH, temperature, incubation time, amount of biomass and analyte, and presence of foreign ions. Methylmercury is immediately bound to the yeast cells over a wide pH and temperature range. The fraction of methylmercury bound was in all cases 100% and was unaffected by the parameters mentioned above. Hg(II) has less affinity for yeast cells and remains in solution, although the percentage of Hg(II) bound to the cell does increase at high incubation time (3 h) and biomass. Of the foreign ions tested, chloride at high concentrations strongly increases the Hg(II) binding efficiency. Methylmercury and Hg(II) are quantitatively separated under optimum conditions, i.e., 30 min incubation time at pH 7.0 and 37 degrees C. The results were compared with those obtained using a purified S. cerevisiae isolate, and no significant differences were observed. Our work suggests that the cell rapidly reduces CH3Hg+ to more volatile species, such as Hg(I) or Hg0, whereas Hg2+ is slowly bound and reduced, perhaps because of the different toxicities of the two species. The method was applied to the selective determination of CH3Hg+ and Hg(II) in spiked water samples. In all cases good recoveries were obtained.

Cations↗

Single-centre experience of peripheral blood stem cell transplantation using cryopreservation by immersion in a methanol bath.

A simplified method to remove and cryopreserve peripheral blood stem cells (PBSC) was utilised to restore the bone marrow in 31 patients with haematological or solid neoplasms after ablative chemotherapy. Mobilization was performed with subcutaneous G-CSF, starting 4 days before the first PBSC harvest and continuing to the last day of harvest. Cryopreservation was carried out by freezing cells to -80 degrees C after addition of autologous fresh plasma with DMSO, in a methanol bath and non-programmed freezer. The PBSC were reinfused in all cases. The mean quantity of CD34 cell (x 10(6)/kg) infused was 6.5 +/- 6.7. The mean number of procedures needed to harvest an appropriate number of PBSC was 3.6 +/- 1.3. The mean times necessary to recover more than 0.5 x 10(9)/l granulocytes were 11 +/- 4 (8-30) days and 23 +/- 13 (8-55) days to obtain more than 20 x 10(9)/l platelets. These results confirm our method as very effective in achieving a high-quality harvest, and it was used in paediatric and adult patients without problems. This procedure, using a non-programmed freezer, simplifies and reduces enormously the cost of the technical measures currently used, enabling their adoption in almost any clinical oncological institution.

Adolescent↗

Evaluation of biological sample mineralisation methods for the determination of fluorine by graphite furnace molecular absorption spectrometry.

Various mineralisation methods were evaluated as means of treating different liquid and solid biological samples for the determination of fluorine by the formation of aluminium monofluoride in an electrothermal graphite furnace and molecular absorption spectrometry (AIF-MAS). Simple sample dilution and the use of 0.01 M Al3+ + 0.01 M Sr2+ solution as a matrix modifier are sufficient to determine the fluorine content in most liquid samples, although some require the addition of 0.3 M ammonium nitrate to the matrix modifier solution in order to diminish background absorbance. In solid samples, treatment methods routinely used with fluoride ion-selective electrodes such as microdiffusion, furnace ashing - microdiffusion and oxygen flask combustion, were tested for compatibility with AIF-MAS. The results were compared with those obtained with a fluoride ion-selective electrode. The proposed mineralisation methods were checked for applicability to different plants, foodstuffs and other biological materials. Some of the methods gave an over-all precision of better than 10%, which is often acceptable, and all methods gave recoveries above 80%. Differences between labile + ionic fluoride and total fluorine can be established by sample treatment.

Evaluation Studies as Topic↗

Evaluation of oxidant media for the determination of lead in food slurries by hydride generation atomic absorption spectrometry.

Several oxidant media were evaluated for the generation of lead hydride from slurry samples and their application to the determination of lead in vegetables and fish by hydride generation atomic absorption spectrometry. Three oxidant - acid media were compared: hydrogen peroxide - nitric acid, ammonium persulphate - nitric acid and potassium dichromate - lactic acid. The powdered samples were suspended in Triton X-100 and shaken with 10.0 g of blown zirconia spheres until a slurry was formed. The potassium dichromate - lactic acid medium was the most satisfactory for the determination of lead in fish and vegetables, providing the lowest detection limits as a result of its high sensitivity and low blank values. The ammonium persulphate - nitric acid medium gave good accuracy, precision and selectivity for vegetables (1-2 p.p.m. of lead); however, with fish (0.1-1 p.p.m. of lead) it was only a semi-quantitative medium for the determination of lead owing to its lack of sensitivity and selectivity. The hydrogen peroxide - nitric acid medium was unsatisfactory for the generation of lead hydride from slurry samples because of decomposition of hydrogen peroxide by the organic matter in the sample.

Food Analysis↗

Degradation of atrazine and several organophosphorus pesticides in oranges.

The degradation of atrazine and four organophosphorus pesticides (chlorpyriphos, fenamiphos, methidathion and methyl-parathion) in oranges was studied. Oranges were immersed in a Milli-Q water solution spiked with 10 mg litre-1 of each pesticide for one day, allowing their adsorption on the orange peel. Then, the oranges were rinsed with Milli-Q water and left outdoors to expose them to natural ambient conditions for two weeks. In parallel, an aqueous solution containing 1 mg litre-1 of each pesticide was placed in a Pyrex flask, which was tightly closed, and exposed to the same ambient conditions. Both samples (orange peel and Milli-Q water) were analyzed periodically by gas chromatography coupled to a nitrogen-phosphorus detector. The pesticide degradation in both samples could be described using a first-order degradation curve. Half-lives varied from 14.5 to more than 30 days in aqueous solution and from 2.3 to 4.1 days in oranges for organophosphorus pesticides, while those for atrazine were 3.1 days and 14.2 days, respectively. The presence of some organophosphorus degradation products in water samples after storage under the above conditions was confirmed by gas chromatography-mass spectrometry.

Atrazine↗