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In this study, we investigated the main constituent, the predominant class and biological activity of the essential oil extracted from the leaves of Pimenta dioica and the pattern of the major constituent against larvae in the third stage of Aedes aegypti. For this reason, we extracted the oil by hydrodistillation, identified its components by gas chromatography coupled with mass spectrometry (GC/MS) and calculated the lethal concentration (LC50) of the larvicidal activity using the Reed-Muench method. The results show that the oil consists mainly of eugenol, in which the phenylpropanoid class predominated and the lethal concentration, LC50, was 38.86 μg mL-1at a confidence level of 2.25 μg mL-1, while the eugenol standard presented LC5079.75 μg mL-1at a confidence level of 2.10 μg mL-1. Given the facts, we conclude that the oil is more active than the standard and that it has the potential to replace chemical larvicides.

This worlk proposes a rapid, sensitive and accurate flow-batch digital image colorimetric (FB-DIC) system to zinc oxid determination in ointments. The method was based on the reaction between Zn(II) ions and zincon at pH = 9.0. The Zn(II)-zincon complex was formed and detected in the mixing chamber. It was designed with two opposite glass windows: one for the webcam and other for the ultra-bright LED. Absorbance was calculated by the norm of the vector in the RGB space. The method had a linear range between 1.0-8.2 mg L–1 with R2 = 0.9998 (n=8) and limit of detection estimated as 5.7 mg L–1. The relative standard deviation (RSD) and sample throughput were estimated at 0.06% and 109 samples h-1, respectively. Ointment commercial samples were analyzed by FB-DIC and the refference method. The results shown no statistically significant difference between them, when was applied the paired t-test at the 95% confidence level. According to green analytical chemistry (GAC) principles the FB-DIC system can be considered eco-driendly due to its low samples and reagents consumption as its low waste generation.

Este trabalho propõe um método colorimétrico por imagens digitais para determinação de metanol em bebidas alcoólicas. O método é baseado na oxidação do metanol a formaldeído, seguido da reação com ácido cromotrópico produzindo um composto púrpura. Imagens digitais do produto de reação são capturadas usando um scanner e as estas são tratadas usando o programa ImageJ. As condições experimentais foram otimizadas e uma curva analítica, usando o índice colorimétrico de imagens digitais como resposta analítica, foi construída na faixa de 0,0100%-0,1000% v/v de metanol. Os limites de detecção e quantificação foram 1,95 x 10-³% e 6,50 x 10-³% v/v, respectivamente. A viabilidade do método é ilustrada na aplicação em amostras de cachaça e licor. Em comparação com a espectrometria ultravioleta-visível, os resultados não mostraram diferenças estatisticamente significativas mediante aplicação do teste-t emparelhado ao nível de confiança de 95%. Em comparação com outros métodos semelhantes, o proposto apresentou uma sensibilidade superior. Tal característica vantajosa é atribuída à natureza trivariada da detecção do scanner.

RESUMO A pesquisa descreve a reação espectrofotométrica do complexo Cu(II)-PAN (1-(2-piridilazo)-2-naftol) e determina a concentração de cobre (II) em aguardente de mandioca (Tiquira). Para isso, dimensionamos a reação para os estudos de absorção do complexo, pH, estabilidade, proporção estequiométrica, interferentes, correlação e recuperação. Após essa etapa, determinamos a concentração de cobre(II) em cinco amostras de bebidas destiladas artesanalmente de cinco municípios do Estado do Maranhão. O resultados mostram que o complexo absorve em 548 nm em pH 6, é estável em um tempo de 7 horas em proporções estequiométrica mínima de 1:1 do ligante e metal, possui limite de detecção em 3,3 X 10-2 mg L-1, faixa de linearidade de 1 X 10-6 a 1 X 10-5 mol L-1, correlação (R2= 0,9990), desvio padrão=0,0035 e recuperação em 104,54 ± 7,01 e os principais íons interferentes são o ferro (III) e o cobalto (II). Na aguardente, constatamos que o teor de cobre está acima do permitido pela legislação brasileira. SUMMARY The search describes the spectrophotometric reaction of the Cu (II)-PAN (1-(2-pyridilazo) -2-naphthol) complex and determines the concentration of copper (II) in manioc spirit (Tiquira). For this, we dimensioned the reaction for the studies of complex absorption, pH, stability, stoichiometric ratio, interferences, correlation, and recovery. After this step, we determined the concentration of copper (II) in five samples of beverages distilled artisanal from five municipalities of the State of Maranhão. The results show that the complex absorbs at 548 nm at pH 6, is stable at a time of 7 hours in minimum 1:1 stoichiometric proportions of the binder and metal, has a detection limit in 3.3 X 10-2 mg L-1, range (R2= 0.9990), standard deviation= 0.0035 and recovery at 104.54 ± 7.0, and the main interfering ions are iron (III) and cobalt (II). In the brandy, we find that the copper content is above that allowed by Brazilian legislation.

A flow-injection spectrometric method for determination of sodium diclofenac in pharmaceutical formulations was developed on this work. Sodium diclofenac solutions were injected into a stream of deionized water that reacted with potassium permanganate on acid medium producing Mn2+ ions whose exhibit maximum absorbance at 450 nm. The methodology used optimize experimental parameters was 33 factorial design and response surface. The proposed method obeyed the Beer’s Law over the range 25-160 mg L-1, applied in tablets and ampoules samples. Results were compare with the reference method. It was verified at the 95% confidence level, through paired t -test application – there is no statistic difference between them. The detection limit was valued in 2.6 mg L-1, relative standard deviation for 10 consecutive injections was 1.5% (100.0 mg L-1 sodium diclofenac solution) and the sample throughput was 80 samples h-1. Regarding optimization of operational conditions, the FIA spectrometric method presented analytical performance as good as other elaborated flow analyzers. Offers a simple and inexpensive way to this drug indirect determination aiming quality control on pharmaceutical industry’s assembly line. However, it can not be used for adulteration screening analysis due to non-selectivity and non-specificity of redox reactions.

This study addresses the challenge of performing fast and accurate titrations with end points that are difficult to identify. In this sense, the combination of digital movies (DMs) with a flow-batch analyzer (FBA) has shown to be a promising analytical tool. In a digital movie-based automatic titrator (DMB-AT), a DM is recorded by a webcam as the titrant is added in the mixing chamber (MC). The DM is then decompiled into frames that are ordered sequentially. In the first frame, the region of interest (ROI) of 257 × 255 pixels is defined. The red (R) component is used to calculate the Pearson's correlation coefficient (r) between the first frame and each subsequent one. The titration curve is obtained in real time by plotting r values and the opening time of the titrant valve. The experimental titration curve is fitted in a sigmoidal regression, and the new titration curve is used to estimate the end point by means of the second derivative method. A software program written in Adobe AIR for a desktop platform programmed in ActionScript 3.0 controlled the opening time of the solenoid valves, gathered the analytical signal and carried out the analytical procedure in real time. The feasibility of the method was confirmed by determining the total hardness and the total alkalinity in mineral waters. The results were compared with classical batch titration and did not exhibit statistically significant differences when the paired t-test at the 95% confidence level was applied. The proposed method is able to process approximately 67 and 86 samples h− 1 for total hardness and total alkalinity, respectively. Its precision was confirmed by overall relative standard deviation (RSD) values of less than 1.0% in both applications.

Neste trabalho foi desenvolvido um sistema de multicimutacao em fluxo para determinacao de diclofenaco de sodio, acido acetilsalicilico e fluoretos em injetaveis, comprimidos e aguas de torneira, respectivamente. Para diclofenaco de sodio o metodo usado foi baseado em sua reacao com permanganato de potassio (20 - 80 mg L -1 ). Para acido acetilsalicilico o metodo usado foi baseado na reacao de Trinder apos hidrolise alcalina do analito (25 - 100 mg L -1 ). Para ions fluoreto o metodo usado foi o bem conhecido SPADNS (0.4 - 1.6 mg L -1 ). Resultados foram comparados com seus respectivos metodos de referencia e, aplicando o teste- t emparelhado, nenhuma diferenca estatisticamente significativa foi verificada entre eles ao nivel de confianca de 95%. Apos a otimizacao das variaveis do sistema analitico, ele foi capaz de analizar 80, 72 e 68 amostras h -1 contendo diclofenaco de sodio, acido acetilsalicilico e fluoretos, respectivamente com geracao de residuos reduzida de acordo com os principios basicos da quimica verde.

portuguesEste trabalho descreveu e comparou quatro estudos entre si que utilizaram metodos automaticos em fluxo com deteccao espectrofotometrica e a reacao de oxidacao do diclofenaco para determinar diclofenaco em formulacoes farmaceuticas 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, conclusoes obtidas e comparamos entre eles os limites de deteccao, desvio padrao relativo e a frequencia analitica. Os resultados mostraram diferencas significativas entre metodos empregados e a utilizacao do Sistema automatico do tipo Analise por Injecao Sequencial, apesar deste possuir menor frequencia analitica. EnglishThis 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.

The pleasant taste and flavor of coffee are responsible for making it one of the most preferred and consumed beverages around the world. Industrial coffee plants usually roast both coffee and adulterants together, which affects directly the quality of the product, specially the sensorial characteristics of the drink. Therefore, this work aims the identification of adulterations in ground roasted coffees (due to the presence of husks and sticks) using ultraviolet–visible spectroscopy and the Successive Projections Algorithm for variable selection in association with Linear Discriminant Analysis (SPA-LDA). For this purpose, extracts of ground roasted coffees prepared in hot water alone (representing the final product as ingested by the consumers) were then analyzed. The proposed methodology obtained a 100% classification in both training and test sets, providing a simple and fast analysis of the aqueous extracts of ground roasted coffees. Moreover, it can also afford security to coffee consumers and regulatory agencies, preventing the fraudulent labeling.

This study proposes a digital image-based flow-batch analyzer (DIB-FBA) for aluminum (III) and chromium (VI) determinations in natural water. A webcam with a CCD sensor and RGB data are used. The method for determining aluminum is based on an Al(III) ion, quercetin, and cetyltrimethylammonium bromide (CTAB) reaction which yields a yellow colored complex in an acetate buffer medium (pH 5.5). The determination of chromium is based on a Cr(VI) ion with 1,5-diphenylcarbazide (DPC) reaction whose product is a violet colored complex. Digital images present the color of the emergent (complementary) radiation to that absorbed by the complexes formed in each analysis. RGB data were employed to build the analytical curves. All standard solutions were prepared in-line, and all analytical processes were completed by simply changing the operational parameters in the DIB-FBA control software. The working ranges were from 10 to 600 μg L − 1 for Al(III) with r = 0.9994 (n = 5), and 10 to 300 μg L − 1 for Cr(VI) with r = 0.999 (n = 5), the limits of detection were 3.97 and 2.65 μg L − 1 respectively for Al(III) and Cr(VI). The relative standard deviation (RSD %) and sampling rate were estimated at 1.5% and 137 h − 1 and at 1.7% and 134 h − 1 for Al(III) and Cr(VI), respectively. Comparing with the reference method, no statistically significant differences were observed when applying the paired t -test at a 95% confidence level.

The traditional flow chemiluminescence (CL) systems typically use flow cells in spiral shape mounted in front of a photomultiplier tube (PMT). The sample is transported by using carrier fluids, undergoes dispersion, and mixes with reagents and CL reaction occurs before reaching the flow cell. As a consequence, the maximum of the chemiluminescence intensity is not exploited and the sensitivity is significantly diminished. In this work, these drawbacks were overcome by using a flow–batch approach and a large area silicon photodiode instead of PMT in order to build a simple and automatic luminometer for CL measurements. The feasibility of the proposed flow–batch luminometer was demonstrated in the determination of vitamin B 12 in injection ampoules, yielding limits of detection and quantification (0.11 and 0.36 μg L − 1 , respectively), recovery rates (between 97.8 and 102.1%), relative standard deviations (RSD − 1 ). Thus, it was possible to both project and build a simple, flexible, versatile and automatic luminometer, while keeping the excellent characteristics of the previous flow–batch analyzer such as: low reagent and sample consumption and minimal waste generation.

A lab-made interface for acquisition of instrumental analog signals between 0 and 5 V at a frequency up to 670 kHz at the parallel port of a microcomputer is described. Since it uses few and small components, it was built into the connector of a printer parallel cable. Its performance was evaluated by monitoring the signals of four different instruments and similar analytical curves were obtained with the interface and from readings from the instrument' displays. Because the components are cheap (~U$35,00) and easy to get, the proposed interface is a simple and economical alternative for data acquisition in small laboratories for routine work, research and teaching.

A new method for metronidazole determination, based on spectrometric monitoring of a diazonium salt produced in-line by alkaline hydrolysis released nitrite ions, was developed and successfully applied to pharmaceutical tablets (r = 0.9993, 2.0-20.0 mg L-1, DL = 0.7 mg L-1) with no interference from common ingredients accompanying the drug. Um novo método para determinação de metronidazol, baseado no monitoramento espectrométrico do sal de diazônio produzido in-line pelos íons nitrito, liberados numa hidrólise alcalina, foi desenvolvido e aplicado com sucesso a comprimidos (r = 0,9993, 2,0-20,0 mg L-1, LD = 0,7 mg L-1), sem interferência de ingredientes comumente presentes.

A microcontrolled, portable and inexpensive photometer is described. It uses six light-emitting diodes (LEDs) as radiation sources and a phototransistor as detector, as well as a microcontroller (PIC - Programmable Controller of Interruption). This device provided total autonomy to the proposed photometer, which was successfully applied to determination of Fe2+ in ferrous syrups and of seven clinical biochemical parameters. As the components are cheap (~U$30.00) and easy to find, the proposed photometer is an economical alternative for routine chemical analyses in small laboratories, for research and teaching. Being portable and microcontrolled, it allows doing field chemical analyses.