Metabolomics analysis of (Geo)propolis from Brazilian stingless bees by FIA and UHPLC-HRMS (Orbitrap).

Native stingless bees (Meliponini) from Brazil make (geo)propolis which is largely used in folk medicine, specially by indigenous and quilombos communities and beekeepers´ families but are progressively being recognized for their pharmacological activities. In this study, the ethanolic extracts of (geo)propolis (EEGs) from Melipona marginata, M. quadrifasciata, M. scutellaris, and Tetragonisca angustula were analysed by Flow injection analysis (FIA) and Ultra-high performance liquid chromatography (UHPLC) in a high resolution Orbitrap mass analyser (HRMS) to investigate and compare their chemical profile. Untargeted metabolomic approach based on UHPLC-HRMS experiments, and bioinformatic tools, allowed to annotate 59 compounds from diverse classes such as: flavonoids, phenolic compounds, sugars, terpenoids, and lipids. In addition, using multivariate tools and Flow injection- high resolution mass spectrometry (FIA-HRMS), it was possible to classify samples and identify marker ions related to the bee species or genus and to the geographical origin as a proof of concept.

Restricted double access ionic imprinted polymer for online extraction and determination of copper from milk samples via FIA-FAAS system.

BACKGROUND: Determining metals in complex biological samples, such as milk, typically involves dry or wet decomposition. However, these techniques have limitations, including low selectivity, risk of contamination, and the use of large reagent volumes. To solve these problems, solid-phase extraction (SPE) using multifunctional sorbents has been extensively explored. In this context, this work proposed synthesizing a new restricted double access ionic imprinted polymer (RAIIP-BSA), for online SPE and determination of Cu2+ from untreated milk samples via flow injection analysis and flame atomic absorption spectrometry (FIA-FASS). RESULTS: Firstly, the polymer was obtained by bulk polymerization using Cu2+ as a template, 4-vinyl pyridine as a functional monomer, and glycidyl methacrylate as a hydrophilic comonomer. Subsequently, it was covered with bovine serum albumin, creating the restricted double access barrier. The obtained material could exclude 97 % of the proteins from milk samples. RAIIP-BSA was chemically and physically characterized. The main extraction variables were optimized via multivariate optimization. The method showed good figures of merit, such as linearity ranging from 0.05 to 1.0 mg L-1, LoD and LoQ of 0.03 and 0.05 mg L-1, intra- and interday precision ranging from 0.73 to 4.14 % and 0.16-3.68 %, and an intra- and interday accuracy ranging from 97.0 to 115.0 % and 103.0-119.0 %, respectively. SIGNIFICANCE: The developed method demonstrates the effective extraction of Cu2+ from untreated milk samples, exhibiting selectivity, high extraction capacity, prolonged sorbent (RAIIP-BSA) durability, simplicity, and swift operation. This method holds promise as an alternative to conventional metal analysis approaches in complex matrices.

Secuelas respiratorias clínicas, funcionales y tomográficas de pacientes hospitalizados por Covid-19 al año del diagnóstico: ESTUDIO SECUELAR-19 / Clinical, functional and tomographic respiratory sequels of patients hospitalized for COVID-19 at one year of diag nosis: SECUELAR-19 TRIAL

Resumen Introducción : Hay información escasa sobre evolución a largo plazo de pacientes hospitalizados por neumo nía COVID-19 moderada (NM) y grave (NG). El objetivo del estudio fue determinar impacto clínico, funcional respiratorio y tomográfico (TACAR) luego del alta a 12 meses del diagnóstico. Métodos : análisis según grupos NM y NG, desatura dores (PD) en prueba de caminata 6 min (PC6M) y patrón tomográfico símil fibrótico (SF). Comparamos resultados a 3 y 12 meses de seguimiento. Resultados : 194 pacientes enrolados, evaluados al año: 103 (53% ): masculinos (62.4%), edad 57.7 ± 10.9 años, comorbilidades (hipertensión arterial 38.8%, dia betes 29.6%, antecedentes respiratorios-AR- 18.4%). Com paramos variables a los 3 y 12 meses (media/DE): CVF 84%(19) a 88(19) (p = 0.01); 27% tuvo CVF<80% al año. En PC6M: 426 metros (108) a 447(92) (p = < 0.01). El 12.8% fue PD al año. NG tuvo mayor SF (40% vs. 27.9% p = 0.021). SF se relacionó con CVF <80% (p = 0.004) en toda la co horte, y NG (p < 0.001). Al año en análisis multivariado se asoció a CVF <80%, AR (OR 4.32, 1.15-16.25), diabetes (OR 2.96, 1.02-8.57) y patrón SF (OR 3.51, 1.25-9.88). PD se asoció a AR (OR 12.2, 2.41-61.85). Discusión : Se observó mejoría en todas las variables al año. Pero al año persisten alteraciones funcionales y tomográficas en <50% de los pacientes. El subgrupo de PD se relacionó a AR. Es importante el seguimiento protocolizado de los pacientes hospitalizados, especial mente los grupos NG, PD y SF.

Abstract Introduction : There is scarce information on longterm evolution of hospitalized patients with moderate (MP) and severe (SP) COVID-19 pneumonia. Objective: to de termine clinical, respiratory function, and tomographic (HRCT) impact after being discharged 12 months after diagnosis. Methods : Analysis according to MP and SP, desatura tor patients (DP) in 6-minute walking test (6MWT) and HRCT fibrotic-like pattern (FLP). Results compared at 3 and 12 months of follow-up. Results : 194 patients enrolled and one year later 103 (53%) were evaluated: gender male (62.4%), age 57.7 ± 10.9 years, comorbidities (arterial hypertension 38.8%, diabetes 29.6%, and respiratory diseases-RD-18.4%). Variables compared 3 months to 12 months (mean/SD): FVC: 84%( 19) to 88%( 19) (p= 0.01). A 27% of patients had FVC<80% at one year. In 6MWT:426 (108) to 447 (92) (p = <0.01). 12.8% are DP in one year. SP had a greater FLP than MP (40% vs. 27.9%, p = 0.021). The FLP group was related to FVC < 80% (p = 0.004) in all patients but only in SP (p < 0.001). After one year, in multivariate analysis, FVC < 80% was associated with RD (OR 4.32, 1.15-16.25), diabetes (OR 2.96, 1.02-8.57) and FLP (OR 3.51, 1.25-9.88). DP were associated with RD (OR 12.2, 2.41-61.85). Discussion : Improvement was observed in all vari ables when comparing 3 to 12 months. However, after one year, functional and tomographic alterations persist in less than 50% of patients. DP subgroup was related to RD. Protocolled follow-up of hospitalized patients is important, especially in SP, DP, and FLP groups.

Simultaneous Determination of Uric Acid and Caffeine by Flow Injection Using Multiple-Pulse Amperometry.

The present study reports the development and application of a flow injection analysis (FIA) system for the simultaneous determination of uric acid (UA) and caffeine (CAF) using cathodically pretreated boron-doped diamond electrode (CPT-BDD) and multiple-pulse amperometry (MPA). The electrochemical profiles of UA and CAF were analyzed via cyclic voltammetry in the potential range of 0.20-1.7 V using 0.10 mol L-1 H2SO4 solution as supporting electrolyte. Under optimized conditions, two oxidation peaks at potentials of 0.80 V (UA) and 1.4 V (CAF) were observed; the application of these potentials using multiple-pulse amperometry yielded concentration linear ranges of 5.0 × 10-8-2.2 × 10-5 mol L-1 (UA) and 5.0 × 10-8-1.9 × 10-5 mol L-1 (CAF) and limits of detection of 1.1 × 10-8 and 1.3 × 10-8 mol L-1 for UA and CAF, respectively. The proposed method exhibited good repeatability and stability, and no interference was detected in the electrochemical signals of UA and CAF in the presence of glucose, NaCl, KH2PO4, CaCl2, urea, Pb, Ni, and Cd. The application of the FIA-MPA method for the analysis of environmental samples resulted in recovery rates ranging between 98 and 104%. The results obtained showed that the BDD sensor exhibited a good analytical performance when applied for CAF and UA determination, especially when compared to other sensors reported in the literature.

Phytochemical profile of petals from black Dahlia pinnata by flow injection analysis-electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry.

INTRODUCTION: Dahlia pinnata Cav. is a flower native to Mexico that has many applications; in particular, its petals have been used for ornamental, food, and medicinal purposes, for example to treat skin rashes and skin cracks. It has been reported that the medicinal properties of plants are generally related to the phytochemical constituents they possess. However, there are few studies on black D. pinnata. OBJECTIVES: The present study was aimed at qualitatively and quantitatively determining the phytochemical profile of petals from black D. pinnata. METHODOLOGY: Phytochemicals from Dahlia petals were extracted by consecutive maceration (hexane, dichloromethane, and methanol); then, the extracts were analyzed through colorimetric assays and UV-Vis spectroscopy for qualitative identification and quantification of phytochemical compounds, respectively. The methanolic extract was analyzed by flow injection analysis-electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry (FIA-ESI-FTICR-MS) in negative and positive mode. RESULTS: Quantitative phytochemical profiling of the methanolic extract by UV-Vis spectroscopy indicated high contents of phenolic compounds (34.35 ± 3.59 mg EQ/g plant) and sugars (23.91 ± 1.99 mg EQ/g plant), while the qualitative profiling by FIA-ESI-FTICR-MS allowed the tentative identification of several flavonoids and phenolic acids. Kaempferol-3-rutinoside, pelargonidin-3-(6″-malonylglucoside)-5-glucoside, rutin, kaempferol-3-(2″,3″-diacetyl-4″-p-coumaroylrhamnoside), and myricetin-3-(2‴-galloylrhamnoside) were the main compounds detected. CONCLUSION: The results expand our knowledge of the phytochemical constituents of petals from black D. pinnata.

Creatine and creatinine quantification in olympic athletes: dried blood spot analysis pilot study.

Capillary dried blood spot (DBS) samples facilitate field-based collection without venipuncture. This pilot study aims to evaluate the viability of creatine (Cr) and creatinine (Crt) quantification using fresh capillary serum (CrS/CrtS) and DBS samples (CrDBS/CrtDBS), using Flow Injection Analysis Mass Spectrometry (FIA - MS). Nine Olympic Athletes provided a capillary blood sample to assess CrS/CrtS and CrDBS/CrtDBS quantified by FIA - MS. No difference between CrtS (mean ± SD: 813.6 ± 102.4 µmol/L) and CrtDBS (812.4 ± 108.1 µmol/L) was observed with acceptable variance [SEM 88.7; CV 10.7%; ICC 0.57 (CI 95% 0.06 - 0.84)] and agreement [very strong (Spearman: r = 0.77; p < 0.01) or strong (Pearson: r = 0.56; p = 0.04); Bland Altman: lower (-193) and upper (+196) limits of agreement]. CrS (mean ± SD: 691.8 ± 165.2 µmol/L) was significantly different to CrDBS (2911 ± 571.4 µmol/L) with unacceptable variance [SEM 171.6; CV 27%; ICC 0.002 (CI 95% -0.02 - 0.07)] and 'weak' agreement [Spearman: r = 0.21, p = 0.47 and Pearson: r = 0.06, p = 0.84; Bland Altman lower (-3367) and upper (-1072) limits of agreement]. Crt quantification is viable using both CrtS and CrtDBS (but not for Cr and CrS/CrDBS), with the DBS tissue handling technique offering several methodological and practice facing advantages. Future work should expand upon the sample size, explore sport/discipline relevant analytes across a full competitive season, including key training, recovery and performance blocks of their periodized performance plan.

Polyphenolic profile by FIA/ESI/IT/MSn and antioxidant capacity of the ethanolic extract from the barks of Maytenus cajalbanica (Borhidi & O. Muñiz) Borhidi & O. Muñiz.

Medium and high polarity extracts from Maytenus species are known to contain polyphenolic compounds such as proanthocyanidins. The high polarity and structural complexity of these compounds make very difficult their isolation even by modern chromatographic techniques. Maytenus cajalbanica (Borhidi & O. Muñiz) Borhidi & O. Muñiz is endemic from Cuba. So far, there are reports neither of phytochemical work nor of biological evaluation of extracts from this subspecies. The goal of this work is to determine the polyphenolic profile and the antioxidant capacity of the ethanolic extract from the barks of Maytenus cajalbanica. FIA/ESI/IT/MSn analysis allowed the identification of 5 flavan-3-ol monomers, 33 proanthocyanidins, 2 free flavonoids and their respective glycosides as major compounds of the ethanolic extract, which showed a strong radical scavenging capacity and a significant ferric reduction power. FIA/ESI/IT/MSn technique led the rapid, effective and sensitive determination of the polyphenolic profile of Maytenus cajalbanica without previous separation.

Utilização dos métodos automáticos em fluxos com detecção espectrofotométrica na determinação de diclofenaco de sódio em formulações farmacêuticas e fluidos corporais / Use of automatic methods in fluxes with spectrophotometric detection in the determination of diclofenac sodium in pharmaceutical formulations and body fluids

RESUMO Este trabalho descreveu e comparou quatro estudos entre si que utilizaram métodos automáticos em fluxo com detecção espectrofotométrica e a reação de oxidação do diclofenaco para determinar diclofenaco em formulações farmacêuticas e fluidos corporais. Para isso, utilizamos os seguintes artigos: Versatility of a multicommuted flow system in the spectrometric determination of three analytes, Sequential injection spectrophotometric method for the assay of anti-inflammatory diclofenac sodium in pharmaceutical preparations, Screening of conditions controlling spectrophotometric sequential injection analysis e Sequential injection spectrophotometric determination of diclofenac in urine and pharmaceutical formulations e detalhamos as metodologias empregadas, os resultados, conclusões obtidas e comparamos entre eles os limites de detecção, desvio padrão relativo e a frequência analítica. Os resultados mostraram diferenças significativas entre métodos empregados e a utilização do Sistema automático do tipo Análise por Injeção Sequencial, apesar deste possuir menor frequência analítica.

SUMMARY This study described and compared four studies that used automatic flow methods with spectrophotometric detection and the oxidation reaction of diclofenac to determine diclofenac in pharmaceutical formulations and body fluids. For this, the following articles were used: Versatility of a multicommuted flow system in the spectrometric determination of three analytes, Sequential injection spectrophotometric method for the assay of anti-inflammatory diclofenac sodium in pharmaceutical preparations, Screening of conditions controlling spectrophotometric sequential injection analysis and Sequential injection spectrophotometric determination of diclofenac in urine and pharmaceutical formulations and we detail the methodologies used, the results, the conclusions obtained and compare the limits of detection, relative standard deviation and analytical frequency. The results showed significant differences between the employed methods and the use of the Automatic System of the Sequential Injection Analysis type, although this one has a lower analytical frequency.

Selective and simultaneous determination of indigo carmine and allura red in candy samples at the nano-concentration range by flow injection analysis with multiple pulse amperometric detection.

A novel, unique electroanalytical method was developed for the simultaneous quantification of the dyes indigo carmine (IC) and allura red (AR) in candies by coupling flow injection analysis and multiple pulse amperometry with a cathodically pretreated boron-doped diamond electrode, using 0.30 mol L-1 H2SO4 as supporting electrolyte. A dual-potential waveform was employed, causing the electrooxidation of either IC solely or IC and AR simultaneously. Thence, subtraction of current signals was used to quantify IC and AR in the concentration ranges of 70.0-1000 nmol L-1 and 40.0-770 nmol L-1, with limits of detection of 40.0 nmol L-1 and 7.0 nmol L-1, respectively. The proposed method, which permits up to 153 determinations per hour with good precision, was successfully applied in the quantification of these dyes in samples of commercial candies; their obtained contents were similar (at a 95% confidence level) to those from a comparative HPLC method.

Ultrasound-assisted dispersive liquid-liquid microextraction of tetracycline drugs from egg supplements before flow injection analysis coupled to a liquid waveguide capillary cell.

A simple, rapid, and efficient ultrasound-assisted dispersive liquid-liquid microextraction (US-DLLME) method was developed for extraction of tetracycline residues from egg supplement samples, with subsequent determination by flow injection analysis (FIA) coupled to a liquid waveguide capillary cell (LWCC) and a controlled temperature heating bath. Tetracyclines react with diazotized p-sulfanilic acid, in a slightly alkaline medium, to form azo compounds that can be measured at 435 nm. The reaction sensitivity improved substantially (5.12-fold) using an in-line heating temperature of 45 °C. Multivariate methodology was used to optimize the factors affecting the extraction efficiency, considering the volumes of extraction and disperser solvents, sonication time, extraction time, and centrifugation time. Good linearity in the range 30-600 µg L(-1) was obtained for all the tetracyclines, with regression coefficients (r) higher than 0.9974. The limits of detection ranged from 6.4 to 11.1 µg L(-1), and the recoveries were in the range 85.7-96.4 %, with relative standard deviation lower than 9.8 %. Analyte recovery was improved by approximately 6 % when the microextraction was assisted by ultrasound. The results obtained with the proposed US-DLLME-FIA method were confirmed by a reference HPLC method and showed that the egg supplement samples analyzed were suitable for human consumption.

Ion Imprinted Polymer for Preconcentration and Determination of Ultra-Trace Cadmium, Employing Flow Injection Analysis with Thermo Spray Flame Furnace Atomic Absorption Spectrometry.

This work proposes a preconcentration method using an ion imprinted polymer (IIP) for determination of cadmium, in several samples, employing a mini-column filled with the polymer coupled into a flow injection analysis system with detection by thermospray flame furnace atomic absorption spectrometry (FIA-TS-FF-AAS). The polymer was synthesized via bulk using methacrylic acid and vinylimidazole as a functional monomer. For the FIA system initial assessment, the variables: pH, eluent concentration and buffer concentration were studied, employing a 23 full factorial design. To obtain the optimum values for each significant variable, a Doehlert matrix was employed. After the optimization conditions as: pH 5.8, eluent (HNO3) concentration of 0.48 mol L-1 and buffer concentration of 0.01 mol L-1, were adopted. The proposed method showed a linear response in the range of 0.081-10.0 µg L-1, limits detection and quantification of 0.024 and 0.081 µg L-1, respectively; preconcentration factor of 165, consumptive index of 0.06 mL, concentration efficiency 132 min-1, and frequency of readings equal to 26 readings h-1 The accuracy was checked by analysis of certified reference materials for trace metals and recovery tests. The obtained results were in agreement with 95% confidence level (t-test). The method was adequate to apply in samples of: jewelry (earrings) (2.38 ± 0.28 µg kg-1), black tea (1.09 ± 0.15 µg kg-1), green tea (3.85 ± 0.13 µg kg-1), cigarette tobacco (38.27 ± 0.22 µg kg-1), and hair (0.35 ± 0.02 µg kg-1).

Evaluation of flow injection analysis method with spectrophotometric detection for the determination of atrazine in soil extracts.

A method for determining atrazine in soil extracts was evaluated by flow injection analysis with spectrophotometric detection. The method is based on the reaction of atrazine with pyridine in an acid medium followed by the reaction with NaOH and sulfanilic acid. Several analytical conditions were previously studied and optimized. Under the best conditions of analysis, the limits of detection and quantification were 0.15 and 0.45 mg L(-1), respectively, for a linear response between 0.50 and 2.50 mg L(-1), and a sampling throughput of 21 determinations per hour. Using the standard addition method, the maximum relative standard deviation of 17% and recovery values between 80 and 100% were observed for three extracts from soil samples with different composition. The proposed method is simple, low-cost and easy to use, and can be employed for studies involving atrazine in soil samples or for screening of atrazine in soils.

Simple and clean determination of tetracyclines by flow injection analysis.

An environmentally reliable analytical methodology was developed for direct quantification of tetracycline (TC) and oxytetracycline (OTC) using continuous flow injection analysis with spectrophotometric detection. The method is based on the diazo coupling reaction between the tetracyclines and diazotized sulfanilic acid in a basic medium, resulting in the formation of an intense orange azo compound that presents maximum absorption at 434 nm. Experimental design was used to optimize the analytical conditions. The proposed technique was validated over the concentration range of 1 to 40 µg mL(-1), and was successfully applied to samples of commercial veterinary pharmaceuticals. The detection (LOD) and quantification (LOQ) limits were 0.40 and 1.35 µg mL(-1), respectively. The samples were also analyzed by an HPLC method, and the results showed agreement with the proposed technique. The new flow injection method can be immediately used for quality control purposes in the pharmaceutical industry, facilitating monitoring in real time during the production processes of tetracycline formulations for veterinary use.

A simple and rapid screening method for sulfonamides in honey using a flow injection system coupled to a liquid waveguide capillary cell.

A rapid and simple screening method was developed for the determination of sulfonamides in honey samples by flow injection analysis (FIA) coupled to a liquid waveguide capillary cell. The proposed method is based on the reaction between sulfonamides and p-dimethylaminocinnamaldehyde (p-DAC) in the presence of sodium dodecylsulate (SDS) in dilute acid medium (hydrochloric acid), with the reaction product being measured spectrophotometrically at λ(max) = 565 nm. Experimental design methodology was used to optimize the analytical conditions. The proposed technique was applied to the determination of sulfonamides (sulfaquinoxaline, sulfadimethoxine, and sulfathiazole) in honey samples, in a concentration range from 6.00 × 10(-3) to 1.15 × 10(-1)mg L(-1). The detection (LOD) and quantification (LOQ) limits were 1.66 × 10(-3) and 5.54 × 10(-3)mg L(-1), respectively. Positive and false positive samples were also analyzed by a confirmatory HPLC method. The proposed system enables the screening of sulfonamides in honey samples with a low number of false positive results, with fast response therefore offers a new tool for consumer protection.

A spectrophotometric flow injection system for streptomycin determination in veterinary samples.

In this work a spectrophotometric flow injection analysis system for streptomycin determination in veterinary samples, is being proposed. The method is based on streptomycin alkaline hydrolysis that forms guanidine, followed by the reaction with Fe(II). The colored product has absorption peak at 520 nm. To evaluate and optimize the system parameters, chemometrics tools, such as factorial design, Pareto chart and Doelhert design, were used. The veterinary samples are diluted in water and introduced in the FIA system, therefore no sample preparation is required. The optimized system presented: linear range of 60 up to 1000 mg L(-1), limit of detection of 18 mg L(-1) and sampling rate of 36 readings per hour. The precision was checked and the CV for veterinary sample readings were always less than 6.5%. The accuracy was studied by comparison with chromatographic method, thus, five samples of pharmaceutical veterinary were determined by HPLC and by the proposed method, and the results are in agreement (t-test, p=0.05).

DESARROLLO DE MÉTODOS DE ANÁLISIS POR INYECCIÓN EN FLUJO A PARTIR DE PROCEDIMIENTOS CLÁSICOS: Determinación de Pb en agua / DEVELOPMENT OF FLOW INJECTION ANALYSIS METHODS BY CLASSICAL PROCEDURES: Determination of Pb in water / DESENVOLVIMENTO DE MÉTODOS DE ANÁLISE POR INJEÇÃO EM FLUXO A PARTIR DE PROCEDIMENTOS CLÁSSICOS: determinação de Pb em água

El análisis químico día a día se acerca más a la automatización, buscando satisfacer las necesidades actuales de resultados rápidos y confiables. Los sistemas de análisis en flujo (FIA - Flow Injection Analysis) son una de las formas de aproximarse a la automatización. En este artículo se presentan los pasos necesarios para implementar una metodología FIA, para la determinación de Pb(II) en agua, partiendo de la revisión de los procedimientos clásicos y describiendo detalladamente los pasos necesarios para implementar la técnica de análisis en flujo. El trabajo produjo un método de análisis de Pb en agua que usa ditizona disuelta en isopropanol (agente cromogénico), en presencia de bromuro de cetiltrimetil amonio (CTAB), para solubilizar en agua el complejo, cuyas características más sobresalientes fueron: volumen de inyección de muestra de 81,7 µL, velocidad de flujo de 8,0 mL/min, tiempo de toma de espectros 1,4 s e intervalo lineal de 1,0 a 40 mg L-1.

Chemical analysis has evolved towards automation to satisfy the current requirements: fast analysis and certainty in the results. Flow injection analysis (FIA) is a way to reach automation. This work presents the necessary steps to obtain an optimized FIA methodology for the determination of Pb(II) in water by classic methods. The result was a FIA method to determinate Pb with dithizone (chromogenic agent) dissolved in iso-propyl alcohol, using cethyltrimethylammonium bromide (CTAB) to solubilize the complex. The main characteristics of the method were: injection sample volume 81.7 µL, flow 8.0 mL/min, spectra acquisition time 1.4 s and linear range 1 to 40 mg L-1.

Cada dia, a análise química é mais cerca da automatização com o fim de satisfazer as necessidades atuais de resultados rápidos e confiáveis. Os sistemas de análise em fluxo (FIA - Flow Inyection Analysis) são uma das formas de aproximação à automatização. Este artigo apresenta os passos necessários para implementar uma metodologia FIA para a determinação de Pb(II) em água, partindo da revisão dos procedimentos clássicos e descrevendo detalhadamente os passos necessários para implementar a técnica de análise em fluxo. Os resultado são um método de análise de Pb em água que usa ditizona dissolvida em isopropanol (agente cromogénico) na presença de bromuro de cetiltrimetil amônio (CTAB), usado para solubilizar o complexo em água. As características principais do método foram: volume de injeção de amostra de 81,7 µL, velocidade de fluxo de 8,0 mL min-1, tempo de aquisição de espectros de 1,4 s e intervalo linear de 0.9 a 40 mg L-1.

Banda de tensão na osteossíntese de côndilo lateral de úmero em um cão / Tension band in osteosynthesis of lateral humeral condyle in a dog

As fraturas de úmero, geralmente, requerem redução cirúrgica para o retorno precoce às suas funções normais de deambulação. O objetivo deste trabalho é relatar uma alternativa na osteossíntese de côndilo lateral do úmero em um cão de pequeno porte. O pino intramedular associado à banda de tensão garante o correto alinhamento dos fragmentos e previne as forças e tração que agem nessa região(AU)

Fractures of the humerus, generally, need a surgical reduction for a prompt return to normal function. The objective of this paper is to relate an alternative in repair of humeral condylar fracture in a small dog. The intramedullary pin associate with tension band guarantees the correct alignment of fragments and prevents the rotation forces and traction that act in this region(AU)

Banda de tensão na osteossíntese de côndilo lateral de úmero em um cão / Tension band in osteosynthesis of lateral humeral condyle in a dog

As fraturas de úmero, geralmente, requerem redução cirúrgica para o retorno precoce às suas funções normais de deambulação. O objetivo deste trabalho é relatar uma alternativa na osteossíntese de côndilo lateral do úmero em um cão de pequeno porte. O pino intramedular associado à banda de tensão garante o correto alinhamento dos fragmentos e previne as forças e tração que agem nessa região

Fractures of the humerus, generally, need a surgical reduction for a prompt return to normal function. The objective of this paper is to relate an alternative in repair of humeral condylar fracture in a small dog. The intramedullary pin associate with tension band guarantees the correct alignment of fragments and prevents the rotation forces and traction that act in this region

Avaliação da atividade bactericida de desinfetantes de uso doméstico, por meio da técnica de análise por injeção em fluxo / Evaluation of the bactericidal activity of disinfectants of domestic use, by means of the technical one of analysis by injection in flow

No presente trabalho a inibição da atividade bactericida foi avaliada através da medida do produto da respiração bacteriana, CO2 utilizando-se a técnica de Análise por Injeção em Fluxo (FIA condutimétrico). Foram utilizadas cepas das bactérias Escherichia coli ATCC 2592 e Staphyloccus aureus ATCC 25923. Como agentes bactericidas foram utilizados cinco marca de desinfetante de fabricação industrial para uso doméstico e três desinfetantes de produção artesanal. De acordo com os resultados os desinfetantes de fabricação industrial demonstraram-se bastante eficientes tanto para E. coli quanto para S. aureus. Os desinfetantes de produção artesanal apresentaram efeito bactericida, para as cepas utilizadas bastante inferior quando comparado aos desinfetantes comerciais.(AU)

In this present assignment, the inhibition of the bactericide activity was evaluated through the measure of thebacterial breathing product, C02 using the technique of Flow Injection Analysis (FIA conductiometric). Samples from Escherichia coli ATCC 2592 and Staphylococcus aureus ATCC 25923 bacteria were used. As bactericide agents were used five commercial disinfectant brands and three home-made production disinfectants. According to the results, the commercial disinfectants demonstrated very efficient to E. coli and also to S. aureus. The home-made production disinfectants showed bactericide effect, to the used samples, quite inferior when compared to the commercial disinfectants. (AU)

Exchangeable aluminum evaluation in acid soils

One of the main factors limiting agricultural production in tropical climate regions is mainly related to the presence of exchangeable aluminum (Al3+) in highly weathered acid soils. Four methods of Al3+ determination extracted with neutral 1 mol L¹ KCl solution were evaluated: three colorimetric methods (aluminon plus ascorbic acid, and eriochrome cyanine R by FIA) and the usual titrimetric method with back-titration. Surface samples from 20 soils of different Brazilian regions, with active acidity (0.01 mol L¹ CaCl2 pH) ranging from very high to medium (3.82 to 5.52), were used. The variance analysis revealed significant interaction among Al3+ determination methods and soil. Mean methods comparisons within each soil (Tukey, P 0.05) indicated that, for most of the soils, the methods differed among each other, although there were high correlations between the obtained values. Al3+ values determined for soil samples by titration varied between 0.15 and 14.71 mmol c dm³. The colorimetric methods showed higher values than the titration method, mainly for those with aluminon (up to 18.75 mmol c dm-3). The Al3+ contents of colorimetric methods correlated quadraticaly with the titration values, for the soil samples with Al3+ > 10 mmol c dm³. Among colorimetric methods, in operational terms, the eriochrome with FIA method presented analytical performance up to 50 samples per hour, easiness and sensibility for routine Al analysis in soil samples. However, due to the specificity, the titration/back-titration method should be used, despite the moroseness, when the Al3+ ions are the objective.

Um dos principais fatores que afetam a produção agrícola em regiões de clima tropical, é a presença de alumínio trocável (Al3+) em solos ácidos altamente intemperizados. Foram avaliados quatro métodos de determinação de alumínio trocável em solução neutra de KCl 1 mol L¹: três métodos colorimétricos (aluminon, aluminon + ácido ascórbico e eriocromo cianina R por FIA) e o método titulométrico usual com retrotitulação ácida. Para obtenção dos extratos de KCl, foram usadas amostras superficiais de 20 solos de diferentes regiões brasileiras, com acidez ativa (pH em CaCl2 0,01 mol L¹) variando de muito alta a média (3,82 a 5,52). A análise de variância revelou interação significativa entre os métodos de determinação e amostras de solos. O teste de médias (Tukey, P 0,05) de métodos dentro de amostras evidenciou, para a maioria das amostras de solos, que os métodos analíticos diferenciaram entre si, embora tenha havido forte correlação entre os valores obtidos. Os valores de Al3+ determinados por titulação variaram de 0,15 a 14,71 mmol c dm³. Os métodos colorimétricos apresentaram valores superiores aos da titulação, notadamente aqueles com aluminon (até 18,75 mmol c dm³). Os teores de Al3+ dos métodos colorimétricos se relacionaram quadraticamente com os teores obtidos por titulação, em amostras de solos com Al3+ > 10 mmol c dm³. Dentre os métodos colorimétricos, o reagente eriocromo cianina R, em sistema FIA, mostrou-se operacionalmente confiável e eficiente para a análise de Al, de amostras de solos, em rotina, com freqüência analítica de 50 determinações por hora. Todavia, devido à especificidade, o método titulométrico com retrotitulação deve ser usado, não obstante a morosidade, quando o objetivo é a determinação do íon Al3+.