Study of macro and microelements in fish from the Cienfuegos Bay. Relationship with its content in sediments.

Thirteen microelements (Al, As, Cd, Co, Cr, Cu, Fe, Li, Mn, Ni, Ti, V, and Zn) and four macroelements (Ca, K, Mg, and Na) were determined in the edible muscle tissue of fish in Cienfuegos Bay. Eight species, Albula vulpes, Diapterus rhombeus, Gerres cinereus, Haemulon carbonarium, Haemulon sciurus, Micropogonias furnieri, Kyphosus sectatrix, and Lutjanus cyanopterus were studied. The total concentrations and extracted concentrations using HCl were also determined in sediments. The quality of the analysis was guaranteed by validating the used analytical methods with certified reference materials of fish and sediments. The high content of macroelements confirmed the importance of fish as a valuable source of food for the local population. New information is provided on bioaccumulation of toxic elements As, Cd, Cu, Zn, and Cr in fish of the bay, with concentrations that overcame the local or international maximum allowable levels for human consumption in most samples analyzed. A high correlation between the content of toxic elements As, Cd, Zn, and macroelement K in fish and its concentration extracted from sediments using the HCl extraction method was observed.

Microwave-assisted digestion of organic samples: how simple can it become?

Advancements in sample preparation for performing trace analysis of inorganic analytes are coming from the dissemination of microwave-assisted procedures, but there is still room for improvements by looking for simple and easily applied procedures. Recently it was proposed a new approach called single reaction chamber with capability for digestions at high pressures and temperatures using simple vials and racks. This was a limitation of former cavity microwave ovens with closed vessels. It was demonstrated here that the use of single reaction chamber approach allows the implementation of efficient digestions using diluted solutions of nitric acid and also allows addressing a critical need of sample preparation for inorganic analysis by running mixed batches of samples. The feasibility of this procedure was demonstrated for organic samples and accuracy was proved by using certified reference materials of apple leaves, bovine liver and whole milk powder. Digestions performed of whole milk powder and bovine liver using 2.0 mol L(-1) nitric acid solution plus concentrated hydrogen peroxide at 240 °C led to residual carbon contents of 0.825 and 1.50% and residual acidities of 1.04 and 0.618 mol L(-1), respectively. These parameters are fully compatible with further measurements using ICP OES or ICP-MS. Al, Cu, Fe, Mn, Mo, Rb, Se, Sr, and Zn were accurately determined by ICP OES or ICP-MS depending on their concentrations in digests.

Focused microwave-induced combustion for digestion of botanical samples and metals determination by ICP OES and ICP-MS.

The advantages and shortcomings of focused microwave-induced combustion (FMIC) for digestion of plant samples were studied. The effects of sample mass, absorbing solution, oxygen gas flow-rate, and time of reflux step on recoveries of major, minor and trace metals were systematically evaluated. Afterwards, Al, Ba, Ca, Co, Cr, Cu, Mg, Mn, Ni, Sr, V, and Zn were determined by inductively coupled plasma optical emission spectrometry (ICP OES) and by inductively coupled plasma mass spectrometry (ICP-MS). The main advantages of FMIC when compared to microwave-assisted wet digestion (MAWD) and focused-microwave-assisted wet digestion (FMAWD) are the possibility to digest larger masses of samples (up to 3g) using shorter heating times and diluted nitric acid solution for absorbing all analytes. Using the selected experimental conditions for FMIC, residual carbon content was lower than 0.7% for all samples and relative standard deviation (RSD) varied from 1.5 to 14.1%. Certified reference materials (NIST 1515 apple leaves and NIST 1547 peach leaves) were used for checking accuracy and determined values for all metals were in agreement with certified values at a 95% confidence level. No statistical difference (ANOVA, 95% of confidence level) was observed for results obtained by FMIC, FMAWD, and MAWD. Limits of detection were lower when using FMIC in the range of 0.02-0.15 µg g(-1) for ICP OES and 0.001-0.01 µg g(-1) for ICP-MS, which were about 3 and 6 times lower than the values obtained by FMAWD and MAWD, respectively. It is important to point out that FMIC was a suitable sample preparation method for major, minor and trace metals by both determination techniques (ICP OES and ICP-MS). Additionally, since it allows lower LODs (because up to 3g of sample can be digested) and diluted acid solutions are used (without any further dilution), the use of ICP-MS is not mandatory.

Sensations and reaction times evoked by electrical sinusoidal stimulation.

OBJECTIVE: To determine whether 5 Hz and 2000 Hz sinusoidal electric currents evoke different sensations and to indirectly evaluate which peripheral nerve fibers are stimulated by these different frequencies. METHODS: One hundred and fifty subjects chose three among eight descriptors of sensations evoked by 5 Hz and 2000 Hz currents and the results were submitted to factor analysis. In 20 subjects, reaction times to 5, 250 and 2000 Hz currents were determined at 1.1 x ST and reaction times to 5 Hz currents were also determined at 2 x ST. RESULTS: Responses were grouped in four factors: Factor 1, which loaded mainly in descriptors related to tweezers stimulation, was higher than the other factors during 2000 Hz stimulation at 1.5 x ST. Factor 2, which loaded mainly in descriptors related to needle stimulation, was higher than the other factors during 5 Hz stimulation. Factor 1 increased and Factor 2 decreased with an increase in 5 Hz intensity from 1.5 to 4x ST. Reaction times measured from the fastest responses were significantly different: 0.57 s (0.16 to 1.60), 0.34 s (0.12 to 0.71) and 0.22s (0.08 to 0.35) for 5, 250 and 2000 Hz, respectively, and 0.22s (0.11 to 0.34) for 5 Hz at 2 x ST. CONCLUSIONS: Sinusoidal electrical stimulation of 5 Hz and 2000 Hz evoke different sensations. At juxta-threshold intensities, RT measurements suggest that 2000 Hz stimulates Abeta-fibers, 250 Hz Abeta- or A partial differential-fibers, 5 Hz Abeta-, A partial differential- or C-fibers. The fiber type, which was initially stimulated by the lower frequencies, depended on inter-individual differences.

Dilute-and-shoot procedure for the determination of mineral constituents in vinegar samples by axially viewed inductively coupled plasma optical emission spectrometry (ICP OES).

Samples of commercial wine vinegar were introduced in an axially viewed inductively coupled plasma optical emission spectrometry instrument (AX-ICP OES) equipped with different sample introduction systems: a cross-flow nebulizer combined with a double-path spray chamber (CF-DP) and cone spray associated with a cyclone spray chamber (CS-CC). Samples of white and red wine vinegar were diluted with water before analysis. Higher magnesium Mg II/Mg I ratios (11 and 10 for CS-CC and CF-DP, respectively) were obtained using a nebulization gas flow rate of 0.6 l min-1 and an applied power of 1.3 kW. The background equivalent concentrations (BEC) and signal-to-background ratio (SBR) of analytes were improved using scandium (Sc) as the internal standard. The limits of detection (LOD) and limits of quantification (LOQ) for mineral constituents were similar for both introduction systems. Best recoveries values were obtained using a plasma under robust conditions, CS-CC system and Sc as the internal standard. The concentration determined in 13 commercial samples of wine vinegars varied between 0.2 and 3.0, between 0.02 and 0.4, between 8.5 and 100.0, between 0.01 and 0.05, between 27.0 and 540.0, between 4.0 and 79.0, between 0.4 and 10.0, and between 0.01 and 2.0 for aluminium (Al), barium (Ba), calcium (Ca), copper (Cu), potassium (K), magnesium (Mg), manganese (Mn), and zinc (Zn), respectively.

The relationship between symptoms and electrophysiological detected compression of the median nerve at the wrist.

OBJECTIVE: The aim of this study was to evaluate the relationship between carpal tunnel syndrome symptoms and compression of the median nerve at the wrist in symptomatic patients. METHODS: A total of 250 patients were selected among those referred for electrodiagnostic evaluation with complaints involving hand or wrist. Primary and secondary symptoms were extracted from the answers to the instrument proposed by Levine et al. [J Bone Joint Surg Am 1993;75:1585]. The association of symptoms and the presence of compression of the median nerve at the wrist were ascertained through a multiple logistic regression test. RESULTS: Secondary symptoms (pain and weakness) were inversely associated with the presence of median nerve compression. Furthermore, primary symptoms (paresthesia, disability and nocturnal symptom) occurred similarly in patients with and without electrophysiologic findings of median nerve compression at the wrist.

On-line pre-concentration of Cr(III) and Mn(II) in FI-FAAS: A critical study involving interference effects and analytical use of an immobilized 8-hydroxyquinoline minicolumn.

A flow injection system with a pre-concentration minicolumn based on a chelating resin was coupled to a flame atomic absorption spectrometer. The focus of this work was the investigation of interference effects and the analytical applicability of the azo-immobilized 8-hydroxyquinoline on controlled-pore glass for the determination of Cr and Mn in mussel and non-fat milk powder. All studied concomitants affected the retention of Cr(III). These effects are probably related to the formation of hydroxo-complexes at the optimum pH range 9.0-10. The positive effect caused by Ca(II) was exploited to increase the retention of Cr(III) species and to improve the slope by 70%. The interferences on Mn(II) retention were less severe. The quantification of Cr and Mn was performed by standard additions. The proposed methodology was validated by analysis of three certified reference materials of mussels (Cr and Mn) and non-fat milk powder (Mn) with a mean relative percent error of <6.5% and mean relative standard deviation of <13%. Chromium and Mn were determined in typical Chilean mussels samples, and Mn was determined in non-fat milk powder samples. Results agreed at the 95% confidence level with those obtained by electrothermal atomic absorption spectrometry (ETAAS) using graphite furnace atomization. The method detection limits for a 30 s pre-concentration time were 0.9 and 1.1 micro g L(-1) for Mn, and 2.2 and 2.5 micro g L(-1) for Cr in acid digested solutions of mussel and non-fat milk, respectively. The methodology is simple, fast (sampling frequency 60-72 h(-1)), reliable, of low cost, and can be applied to the determination of traces of Cr (> or =0.18 micro g g(-1)) and Mn (> or =0.6 micro g g(-1)) in mussel samples, and Mn (> or =0.37 micro g g(-1)) in non-fat milk powder.

Determination of Cd and Pb in food slurries by GFAAS using cryogenic grinding for sample preparation.

A simple method combining slurry sampling after cryogenic grinding and the use of a permanent modification of the integrated platform inside the transversely heated graphite atomizer (THGA) was proposed for the determination of Cd and Pb in foods. Potentialities of the cryogenic grinding were evaluated for grinding different materials of difficult homogenization such as high fat and high fiber tissues. Animal and vegetal samples were cut into small pieces and ground in liquid nitrogen for 2 min. Slurries were prepared directly in the autosampler cup after cryogenic grinding by transferring an exact amount of homogeneous powdered material (5-20 mg) to the cup, followed by 1.00 mL of 0.2% (v/v) HNO3 containing 0.04% (v/v) Triton X-100 and sonication for 30 s, before transferring into the platform previously coated with 250 microg W and 200 microg Rh. Use of a tungsten carbide-rhodium permanent modifier combined with NH4H2PO4 conventional modifier improves tube lifetime and increases the pyrolysis temperature for Cd. Homogeneity tests, carried out by comparing the between- and within-batch precision for each kind of sample, showed no significant differences at the 95% confidence level, indicating good homogeneity for 5-20 mg masses. Detection limits were 3.3 ng g(-1) Cd and 75 ng g(-1) Pb for 1% m/v slurries. Results for determination of Cd and Pb in foods slurries were in agreement with those obtained with digested samples, since no statistical differences were found by the paired t-test at the 95% level.

[A review of technical and physiological aspects of F-wave studies and analysis of the data obtained in a group of diabetic patients]. / Revisão relacionada a alguns aspectos técnicos e fisiológicos das ondas F e análise dos dados obtidos em um grupo de indivíduos diabéticos.

We reviewed some physiological aspects of the F-wave studies, mainly related to the motoneurone sizes involved in the generation of this potentials and the number of stimuli necessary to analyze the F-wave parameters. F-wave latencies and F-wave conduction velocities obtained in a group of normal volunteers and in a group of diabetic patients are analyzed.

A comparison between different parameters in F-wave studies.

Ulnar nerve F-waves were studied in 23 healthy volunteers and 27 diabetic patients. Latencies and chronodispersion were analyzed in each group. In the diabetic group all the parameters were normal in 14 patients (52%) and in 13 (48%) at least one parameter was altered. In these patients the most frequently altered parameter was the maximum latency (92%), followed by mean latency (85%), minimum latency (54%) and chronodispersion (54%). These findings suggest that maximum and mean latencies are better parameters to be analyzed in ulnar F-wave studies than minimum latency.

Focused-microwave-assisted reaction in flow injection spectrophotometry: a new liquid-vapor separation chamber for determination of reducing sugars in wine.

The usefulness of an unsegmented liquid/vapor phases flow injection system for determining reducing sugars in wines using a focalized poly(tetrafluoroethylene) (PTFE) coiled reactor positioned at the output antenna of a domestic microwave oven at 700 W is demonstrated. In this system, sample or reference solution is mixed to 2.5 mol l(-1) sodium hydroxide and 6.8 mmol l(-1) potassium hexacyanoferrate(III) solutions previously merged in a confluence point and the reducing sugars (glucose plus fructose) were oxidized by potassium hexacyanoferrate(III) solution into the PTFE coiled reactor positioned in the microwave oven cavity. After phases separation at a proposed separation chamber (SC), the decrease of K(3)Fe(CN)(6) concentration in the liquid phase was measured at 420 nm. Using this SC, a favorable dispersion profile and a decrease of hydrodynamic pressure were observed. The flow procedure presented similar sensitivities to glucose and fructose in the experimental conditions adopted, allowing the determination of the reducing sugars content (fructose plus glucose concentrations) in the concentration range from 40 to 400 mumol l(-1) with a detection limit of 9 mumol l(-1). The RSD was 1.9% for a 120 mumol l(-1) fructose solution (n=12) and the analytical frequency was 54 h(-1). The results obtained for reducing sugars in several wines using the proposed flow system and those obtained using the Somogyi-Nelson batch procedure were in agreement at the 95% confidence level.

Determination of dysprosium and europium in sheep faeces by graphite furnace and tungsten coil electrothermal atomic absorption spectrometry.

Tungsten coil atomizer atomic absorption spectrometry (TCAAS) was used to determine Dy and Eu in acid-digested faeces of sheep. These elements were used as markers in animal nutrition studies. Samples were dried, ground and decomposed using a nitric-perchloric acid mixture. The accuracy of the developed method was evaluated by graphite furnace atomic absorption spectrometry (GFAAS). The results obtained for Eu were validated at a 95% confidence level using a paired t-test. The results for Dy were not validated owing to memory effects caused by carbide formation into the graphite tube. This effect did not occur for Eu. The detection limits for Dy and Eu were 6.9 and 2.1 mug l(-1) by TCAAS, and 2.2 and 5.2 mug l(-1) by GFAAS, respectively. Relative standard deviations (R.S.D.; n=5) were 0.7-3.8 and 0.8-5.6% for Dy and Eu by TCAAS and 0.8-5.4 and 0.3-3.8% for Dy and Eu by GFAAS, respectively. The lifetime of the tungsten coil was around 200 heating cycles, which is three-fold higher than graphite tube lifetime. The proposed method can be used to determine the passage rate of feed through animal digestive tract.

An attempt to correlate fat and protein content of biological samples with residual carbon after microwave-assisted digestion.

The residual carbon content of a variety of bovine-derived samples and forage was determined by inductively coupled plasma optical emission spectrometry with radial view configuration (ICP-OES) after microwave-assisted digestion under high pressure in a closed vessel. The original carbon concentration in the samples was determined by elemental analysis. The highest amount of original carbon content (64%) was found in viscera. After digestion, up to 75% of it was destroyed. Viscera presented the highest ether extract and blood exhibited a high crude protein content of up to 99%. The efficiency in destroying the organic matter in biological materials seemed to be related to their fat content and showed no significant difficulty for protein-rich samples. The correlation coefficient between the fat content of the samples and the residual carbon after acid decomposition was 0.9173 indicating a fair fit. However, no correlation was observed between % RC and the protein content.

Single vessel procedure for acid-vapour partial digestion in a focused microwave: Fe and Co determination in biological samples by ETAAS.

A single vessel procedure using a focused microwave oven is proposed for biological sample preparation with nitric acid vapour under atmospheric pressure. A laboratory-made PTFE support vessel equipped with four cups that received the samples was adapted to fit on the microwave glass vessel. Biological samples (30 mg) were directly weighed into these PTFE cups followed by the addition of 150 microliters of water or H2O2. The mixture was exposed to acid vapour stemming from 15 ml of concentrated HNO3 placed in the bottom of the glass vessel. The acid vapour was formed at 115 degrees C and brought about the Co and Fe extraction in 10 and 60 min, respectively. The resulting suspension was diluted with 0.14 mol l-1 HNO3 to a final volume of 1.0 ml, shaken and centrifuged. The supernatant was analysed by electrothermal atomic absorption spectrometry (ETAAS) by placing the cups directly in the autosampler of the spectrometer. This system minimised contamination, and reagent and time consumption and was suitable for Co and Fe determination in biological materials. The accuracy of the proposed method was assessed by using certified reference materials and by comparison with the closed vessel microwave as a comparative technique. Cobalt and Fe recovery was around 82-99%. As an additional advantage, up to 6 samples can be simultaneously prepared in each vessel, thereby improving the sample throughput from 6 to 24, when a 6-cavity focused microwave is used.

F-waves and conduction velocities range.

A controversial aspect in F-wave studies is if these potentials are generated preferentially by large motoneuron or by motoneuron of all sizes. The purpose of this work is to compare the maximum and minimum conduction velocities of the fibers that generate the M-wave with the maximum and minimum conduction velocities of the F-waves elicited by ulnar nerve stimulation. There were no significant differences between maximum velocities. However, minimum F-wave velocity was significantly higher than minimum conduction velocity, suggesting that the F-waves registered were preferentially generated by the fastest conducting axons.

Quantitative analysis of EEG background activity in patients with rolandic spikes.

OBJECTIVE: The aim was to compare the background activity, through quantitative EEG analysis, of patients with rolandic spikes and normal age-matched controls. MATERIAL AND METHODS: Twenty-one channel EEG of 23 children with rolandic spikes and 39 normal children, with ages ranging from 7 to 12 years, were submitted to quantitative analysis (FFT) of discharge-free epochs. Patients and controls were divided in groups according to age (7-9 and 10-12 years old). Delta, theta, alpha and beta frequency ranges were compared between groups for all electrode positions. RESULTS: Comparing normals, the 7-9 years old group showed power reduction in the alpha and beta ranges. Comparing patients and normal age-matched groups, the patients showed power increase, at all frequency ranges in the 7-9 years old group and at delta and theta frequency ranges in the 10-12 years old group. CONCLUSIONS: Our findings agree with recent evidences that these children may differ from normal (besides the eventual occurrence of seizures); but they also suggest that these differences can be related to immaturity and not necessarily related to the epileptiform discharge.

Nerve conduction study of the medial and lateral plantar nerves.

The medial and lateral plantar nerves may be evaluated through the recordings of the compound sensory nerve action potentials (CSNAP), compound mixed nerve action potentials (CMNAP) and compound muscular action potentials (CMAP). As some of these potentials are not easily and always obtainable in normal individuals, our purpose was to verify the consistency of these potentials for the study of these nerves. Fifty-one normal adult volunteers were examined. The CSNAP, CMNAP and CMAP, related to the medial and lateral plantar nerves were evaluated bilaterally. CSNAP were not obtained in 7.8% and in 17.6% from the medial and lateral plantar nerves respectively. CMNAP from the lateral plantar nerve were not obtained in 15.6%. CMNAP from the medial plantar nerves and CMAPs from the abductor hallucis and abductor digiti quinti were obtained for all nerves tested. Our results, therefore, suggest that these last 3 parameters are the ones more reliable for clinical application.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution.

A flow-injection system with a Chelite-S(R) cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl(2), in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury to the flow cell in the forward direction or removes the residue from reactor/gas-liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h(-1) (50.0-500 ng l(-1)), consuming about 10 ml sample and 5 mg SnCl(2) per determination. The detection limit is 0.8 ng l(-1) and the relative standard deviation (RSD) (n=12) of a 76.7 ng l(-1) sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found.

Sample size and the study of F waves.

Ulnar nerve F waves were studied in 23 healthy volunteers and 27 diabetic patients. Latencies and chronodispersion were analyzed in each group for different sample sizes. Significant differences were not detected with the different sample sizes for mean latencies, with samples above 16 stimuli or 10 waves for minimum and maximum latencies and above 20 stimuli or 16 waves for chronodispersion. These findings suggest that these limits may be adequate for group comparison. However, for the analysis of individual patients, the evidence suggests that larger samples are required for the determination of the minimum and maximum latencies and chronodispersion.

Median nerve SEP after a high medullary lesion. Preserved N18 and absent P14 components. Case report.

Median nerve SEPs recorded from a patient with a high medullary lesion are described. The lesion involved the anteromedial and anterolateral right upper third of the medulla, as documented by MRI. Forty one days after the lesion, left median nerve SEP showed preserved N18 and absent P14 and N20 components; stimulation of the right median nerve evoked normal responses. These findings agree with the proposition that low medullary levels are involved in the generation of the N18 component of the median nerve SEP.