Influência da calcinação sobre a remoção de ferro da caulinita e ilita e seus efeitos sobre a acidez

Samples of natural clay composed by kaolinite, illite, goethite and quartz, were calcinated and submitted to lixiviation with citrate and chloridric acid in order to remove iron. Investigation due to extraction consequences was carried cut by analyzing its acid properties using ammonia gas as probe in infrared spectrophotometry analysis. The sample that were treated with citrate followed by acid lixiviation yield materials twice more acid than samples treated with acid only.

Determinação potenciométrica em fluxo de cloreto de cetilpiridinio em desinfectantes bucais

The work describes a new procedure for cetylpyridinium chloride determination in oral disinfectants, based on a flow-injection system with potentiometric detection. The determination was based on the measurement of picrate concentration decrease as result of ion-pair reaction with the analyte present in the injected sample. In the optimised set-up the sample injection volume was kept at 400 µL and merged downstream with the reagent solution containing 1,0 x10-5 mol/L of picrate adjusted to pH 5.0 with citrate/citric acid buffer. The flow rate was fixed at 8 mL/min and the reactor length at 40 cm. The proposed procedure enables the determination of cetylpyridinium in the analytical range of 5,0x10-6 - 7,5x10-5 mol/L at a sampling rate of 60/h. The results for real samples had a precision better than 3% and were comparable to the labelled values.

Validation and statistical analysis of two high performance liquid chromatography methods for the determination of indinavir sulfate raw material and capsules

Two high performance liquid chromatography (HPLC) methods for the quantitative determination of indinavir sulfate were tested, validated and statistically compared. Assays were carried out using as mobile phases mixtures of dibutylammonium phosphate buffer pH 6.5 and acetonitrile (55:45) at 1 mL/min or citrate buffer pH 5 and acetonitrile (60:40) at 1 mL/min, an octylsilane column (RP-8) and a UV spectrophotometric detector at 260 nm. Both methods showed good sensitivity, linearity, precision and accuracy. The statistical analysis using the t-student test for the determination of indinavir sulfate raw material and capsules indicated no statistically significant difference between the two methods.

Otimização do banho eletrolítico da liga Fe-W-B resistente à corrosão

A study on optimization of bath parameters for electrodeposition of Fe-W-B alloys from plating baths containing ammonia and citrate is reported. A 2³ full factorial design was successfully employed for experimental design analysis of the results. The corrosion resistance and amorphous character were evaluated. The bath conditions obtained for depositing the alloy with good corrosion resistance were: 0.01 M iron sulfate, 0.10 M sodium tungstate and 0.60 M ammonium citrate. The alloy was deposited at 12% current efficiency. The alloy obtained had Ecorr -0.841 V and Rp 1.463 x 10(4) Ohm cm². The deposit obtained under these conditions had an amorphous character and no microcracks were observed on its surface. Besides this, the bath conditions obtained for depositing the alloy with the highest deposition efficiency were: 0.09 M iron sulfate, 0.30 M sodium tungstate and 0.50 M ammonium citrate. The alloy was deposited at 50% current efficiency, with an average composition of 34 wt% W, 66 wt% Fe and traces of boron. The alloy obtained had Ecorr -0.800 V and Rp 1.895 x 10³ Ohm cm². Electrochemical corrosion tests verified that the Fe-W-B alloy deposited under both conditions had better corrosion resistance than Fe-Mo-B.

Métodos de extração para quantificação de manganês disponível em fertilizantes

The solubility of Mn in different fertilizers (MnSO4.H2O-p.a., MnO2-p.a.+MnO-Ind., MnO2-Ind.+MnO-Ind., MnO2-p.a., MnO2-Ind. and MnO-Ind.) was determined using different methodologies: total content and soluble contents in water, 10% H2SO4, citric acid at 20 g L-1, diluted neutral ammonium citrate, (1+9) and DTPA at 0.005 mol L-1. The Mn solubilities in the latter three extractors were assessed after agitation of the sample for one hour and after boiling for 5 minutes. The extraction procedure using neutral ammonium citrate (1+9), at 1:100, with agitation for one hour, was shown to be the most adequate to assess the availability of Mn in fertilizers.

Determinação espectrofotométrica de citrato de sildenafil em formulações farmacêuticas

This paper describes a simple and rapid spectrophotometric method for quantitative determination of sildenafil citrate based on its reaction with p-chloranil accelerated by hydrogen peroxide, producing a stable purple compound (λmax= 535 nm). In the absence of peroxide this reaction is very slow. The experimental conditions were optimized by using response surface methodologies. Beer's law is obeyed in a concentration range of 8.52 x 10-5 - 1.70 x 10-3 mol L-1 (r = 0.999). The detection limit was 1.96 x 10-5 mol L-1. The method was successfully applied for the determination of sildenafil citrate in medicines with good accuracy and precision.

Determinação de citrato de sildenafila e de tadalafila por cromatografia líquida de ultraeficiência com detecção por arranjo de diodos (CLUE-DAD)

A simple ultra-performance liquid chromatographic method for the simultaneous determination of sildenafil citrate and tadalafil was developed and validated. Sample preparation was dissolution in methanol, followed by centrifugation and dilution (1:10) with methanol. Analysis was performed in an Acquity® UPLC system with Acquity® BEH C18 column (2.1 x 50 mm, with 1.7 μm particles). The elution was isocratic with phosphate buffer pH 2.3 and acetonitrile (65:35, v/v) at a flow rate of 0.7 mL/min. The method presented adequate specificity, linearity, precision and accuracy and allowed the determination of the drugs in seized forensic samples.

Método QuEChERS para determinação de ocratoxina a e citrinina em arroz e farelo de arroz

The present study was carried out to establish the optimal conditions for performing ochratoxin A (OTA) and citrinin (CIT) extraction using the QuEChERS method in rice. Employing the factorial experimental design, variables that significantly influenced the extraction stages were determined. The following variables were analyzed: addition of water, acidification of acetonitrile with glacial acetic acid, as well as amounts of magnesium sulfate, sodium acetate, sodium citrate and diatomaceous earth. The best combining procedure resulted in a predictive model using more water and less diatomaceous earth. Recoveries of CIT and OTA were 78-105%.

Preparação de nanopartículas de prata e ouro: um método simples para a introdução da nanociência em laboratório de ensino

A new practical experiment involving silver and gold nanoparticle syntheses was introduced in an inorganic chemistry laboratory course for undergraduate students at the Institute of Chemistry, UNICAMP. The nanoparticles were synthesized by the reduction of silver nitrate and tetrachloroauric acid with sodium borohydride and sodium citrate in an aqueous medium. Stabilities of the suspensions were tested using several different reactants including sodium chloride, polyvinylpyrrolidone, polyvinyl alcohol and cistamine. Changes in optical properties were observed by electronic spectra and also by transmission electronic microscopy, which also yielded data for estimating particle size.

EVALUATION OF A BUFFERED SOLID PHASE DISPERSION PROCEDURE ADAPTED FOR PESTICIDE ANALYSES IN THE SOIL MATRIX

An evaluation of the pesticides extracted from the soil matrix was conducted using a citrate-buffered solid phase dispersion sample preparation method (QuEChERS). The identification and quantitation of pesticide compounds was performed using gas chromatography-mass spectrometry. Because of the occurrence of the matrix effect in 87% of the analyzed pesticides, the quantification was performed using matrix-matched calibration. The method's quantification limits were between 0.01 and 0.5 mg kg-1. Repeatability and intermediate precision, expressed as a relative standard deviation percentage, were less than 20%. The recoveries in general ranged between 62% and 99%, with a relative standard deviation < 20%. All the responses were linear, with a correlation coefficient (r) ≥0.99.

Direct and simultaneous spectrophotometric determination of Ni (II) and Co (II) using diethanoldithiocarbamate as complexing agent

A direct spectrophotometric method for simultaneous determination of Co(II) and Ni(II), with diethanoldithiocarbamate (DEDC) as complexing agent, is proposed using the maximum absorption at 360 and 638 nm (Co(II)/DEDC) and 390 nm (Ni/DEDC). Adjusting the best metal/ligand ratio, supporting eletrolite, pH, and time of analysis, linear analytical curves from 1.0 10-6-4.0 10-4 for Co(II) in the presence of Ni 1.0 10-6-1.0 10-4 mol L-1 were observed. No further treatment or calculation processes have been necessary. Recoveries in different mixing ratios were of 99%. Interference of Fe(III), Cu(II), Zn(II) and Cd(II), and anions as NO3-, Cl-, ClO4-, citrate and phosphate has been evaluated. The method was applied to natural waters spiked with the cations.

Method to obtain platelet-rich plasma from rabbits (Oryctolagus cuniculus )

Abstract: Platelet-rich plasma (PRP) is a product easy and inxpesnsive, and stands out to for its growth factors in tissue repair. To obtain PRP, centrifugation of whole blood is made with specific time and gravitational forces. Thus, the present work aimed to study a method of double centrifugation to obtain PRP in order to evaluate the effective increase of platelet concentration in the final product, the preparation of PRP gel, and to optimize preparation time of the final sample. Fifteen female White New Zealand rabbits underwent blood sampling for the preparation of PRP. Samples were separated in two sterile tubes containing sodium citrate. Tubes were submitted to the double centrifugation protocol, with lid closed and 1600 revolutions per minute (rpm) for 10 minutes, resulting in the separation of red blood cells, plasma with platelets and leucocytes. After were opened and plasma was pipetted and transferred into another sterile tube. Plasma was centrifuged again at 2000rpm for 10 minutes; as a result it was split into two parts: on the top, consisting of platelet-poor plasma (PPP) and at the bottom of the platelet button. Part of the PPP was discarded so that only 1ml remained in the tube along with the platelet button. This material was gently agitated to promote platelets resuspension and activated when added 0.3ml of calcium gluconate, resulting in PRP gel. Double centrifugation protocol was able to make platelet concentration 3 times higher in relation to the initial blood sample. The volume of calcium gluconate used for platelet activation was 0.3ml, and was sufficient to coagulate the sample. Coagulation time ranged from 8 to 20 minutes, with an average of 17.6 minutes. Therefore, time of blood centrifugation until to obtain PRP gel took only 40 minutes. It was concluded that PRP was successfully obtained by double centrifugation protocol, which is able to increase the platelet concentration in the sample compared with whole blood, allowing its use in surgical procedures. Furthermore, the preparation time is appropriate to obtain PRP in just 40 minutes, and calcium gluconate is able to promote the activation of platelets.

A new allele of peptidase-B in cattle

Electrophoretic analyses of peptidase-B were carried out on red cell hemolysates from Holstein, Mantiqueira and Gyr cattle, using cornstarch, known in Brazil as Penetrose-30. We describe a new peptidase-B allele, denoted Pep-B1, in Mantiqueira cattle, belonging to the Bos taurus group, which are the result of a cross of native cattle of Portuguese origin introduced in Brazil during colonial times (16th century) with Holstein and Caracu cattle. The genetic control of peptidase-B was determined by typing parents and progeny segregating for all three alleles, confirming that peptidase B is controlled by a single autosomal locus with three codominant alleles, denoted Pep-B1, Pep-B2 and Pep-B3 The use of the citrate-phosphate buffer system, at pH 5.9, on 14% gel, under the electrophoretic conditions standardized in this study permitted good visualization of all peptidase-B variants.

Effect of FSH and insulin on lipogenesis in cultures of Sertoli cells from immature rats

Follicle-stimulating hormone (FSH) and insulin regulate glycide metabolism in Sertoli cells, thus stimulating lactate production. These stimulatory effects of FSH and insulin do not require protein synthesis, suggesting a modulation of enzyme activity and/or regulation of glucose transport. The present investigation was performed to characterize the hormonal control of lipid metabolism in Sertoli cells. The data indicate that FSH and insulin have a regulatory effect on lipid metabolism in Sertoli cells. After 8 h of preincubation with insulin (5 µg/ml), the activity of the enzyme ATP-citrate lyase in cultured Sertoli cells was increased from 0.19 to 0.34 nmol NAD+ formed µg protein-1 min-1. FSH (100 ng/ml) had no effect on this enzyme. Glycerol phosphate dehydrogenase activity was not affected by any of the hormones tested. When Sertoli cells from 19-day old rats were incubated with [1,2­14C]acetate for 90 or 360 min, the [14C] label was present predominantly in triglyceride and phospholipid fractions with minor amounts in other lipids. In Sertoli cells pretreated for 16 h with insulin and FSH, an increase in acetate incorporation into lipids was observed. Most of the label was in esterified lipids and this percentage increased with the time of treatment; this increase was remarkable in triglycerides of control cells (18.8% to 30.6%). Since Sertoli cell triglycerides participate in the control of spermatogenesis, the present data suggest that the hormonal control of lipid metabolism in Sertoli cells is important not only for maintaining the energy of the cell itself, but also for the control of the spermatogenesis process.

Isoenzyme analysis of Arthrobotrys, a nematode-trapping fungus

Extraction and isoenzyme analysis of four isolates of Arthrobotrys including A. musiformis, A. robusta and A. conoides were conducted. Among the 14 enzymes studied by starch gel electrophoresis, using morpholine-citrate as gel/electrode buffer, the following nine enzymes showed interpretable banding patterns: a-esterase, fumarase, hexokinase, isocitrate dehydrogenase, leucine aminopeptidase, malate dehydrogenase, 6-phosphogluconate dehydrogenase, phosphoglucomutase and phosphoglucoisomerase. All isolates studied displayed typical isoenzyme phenotypes for each species. Two isolates of A. conoides differed in their a-isoesterase banding patterns, but no differences were observed for the other enzymes. The assay was satisfactory for enzyme extraction and resolution of Arthrobotrys and could be used in future taxonomic and genetic studies of this organism