A green methodology was developed for the extraction and determination of lauryl ether sulfate in raw materials and commercial liquid soap and shower gel samples. The method avoids the use of organic solvents, offering a simple, cheap, and safe analysis. The methodology is based on the sorption of an ionic pair consisting of a cationic dye and an anionic surfactant onto polyurethane foam. The experimental variables were optimized by chemometry to obtain the conditions that maximized extraction of the ionic pair. Digital imaging and spectrophotometry were used for quantification in the linear concentration range from 10.0 to 100 mg L-1. The limits of detection and quantification were, respectively, 2.71 and 9.28 mg L-1 for digital imaging, and 1.74 and 5.83 mg L-1 for spectrophotometry. The methods showed good results when applied to commercial samples, with recoveries in the range 96.8-103%.

A simple, inexpensive, and clean methodology employing a combined spot test/diffuse reflectance spectroscopy procedure was developed and applied for the quality control analysis of lead in hair dyes, using a filter paper platform. The method is based on the complexation reaction of lead, present in a pH 2.8 buffer medium containing tartaric acid and sodium and potassium tartrate, with sodium rhodizonate (ROD) in an aqueous medium containing sodium dodecyl sulfate (SDS) surfactant, yielding a colored compound on the surface of a filter paper. The concentrations of ROD and SDS were optimized using experimental design. The linear range obtained for reflectometric measurements carried out at 545 nm was 4.70-140 mg L-1 of lead (R = 0.998), and the limits of detection and quantification were 1.12 and 3.75 mg L-1, respectively. The proposed method was successfully applied to the analysis of lead in progressive hair dyes.

Um método espectrofotométrico simples, rápido, exato e barato foi desenvolvido para a determinação de tetraciclina e doxiciclina. O método é baseado na reação entre estas drogas e cloramina-T em meio alcalino produzindo produtos de cor vermelha com absorbância máxima em 535 e 525 nm para a tetraciclina e doxiciclina, respectivamente. As melhores condições para as reações foram encontradas utilizando métodos multivariados. A lei de Beer é obedecida no intervalo de concentração de 1,03 x 10-5 a 3,61 x 10-4 mol L-1 e 1,75 x 10-5 a 3,48 x 10-4 mol L-1 para a tetraciclina e doxiciclina, respectivamente. Os limites de quantificação foram 5,63 x 10-6 mol L-1 e 7,12 x 10-7 mol L-1 para a tetraciclina e doxiciclina, respectivamente. O método proposto foi aplicado com êxito na determinação destas drogas em formulações farmacêuticas e os resultados obtidos estão de acordo com os obtido pelo método comparativo em 95% de confiança.

A simple, rapid, accurate and inexpensive spectrophotometric method for the determination of tetracycline and doxycycline has been developed. The method is based on the reaction between these drugs and chloramine-T in alkaline medium producing red color products with absorbance maximum at the Λ = 535 and 525 nm for the tetracycline and doxycycline, respectively. The best conditions for the reactions have been found using multivariate method. Beer´s law is obeyed in a concentration ranges 1.03 x 10-5 to 3.61 x 10-4 mol L-1 and 1.75 x 10-5 to 3.48 x 10-4 mol L-1 for the tetracycline and doxycycline, respectively. The quantification limits were 5.63 x 10-6 mol L-1 and 7.12 x 10-7 mol L-1 for the tetracycline and doxycycline, respectively. The proposed method was successfully applied to the determination of these drugs in pharmaceutical formulations and the results obtained were in good agreement with those obtained by the comparative method at the 95% confidence level.

This paper reports an analytical method for the determination of ambroxol in micellar medium by spot test-diffuse reflectance spectroscopy. The reflectance measurements were performed analyzing the colored compound (λ= 520 nm) produced from the reaction between ambroxol and p-dimethylaminocinnamaldehyde on the surface filter paper. The linear range was from 1.21 × 10"3 to 9.65 × 10"3 mol L-1 (500 - 4000 μg mL-1). The limit of detection and quantification were 3.50 x 10-4 mol L-1 (145 μg mL-1) and 1.16 x 10-3 mol L-1 (481 μg mL-1), respectively. Five commercial samples were analysed and the results obtained by the proposed method were in good agreement with those obtained by the literature method at 95% confidence level.

A flow-injection (FI) spectrophotometric procedure is proposed for tetracycline (TC) and doxycycline (DXC) determination in pharmaceuticals. The method is based on the reaction of oxidation of these drugs by chloramine-T in alkaline medium producing red color products (λmax = 535 and 525 nm). Beer´s law is obeyed in the concentration range from 6.62 x 10-5 to 7.72 x 10-4 mol L-1 and 5.37 x 10-5 to 7.16 x 10-4 mol L-1 for TC and DXC, respectively. The analytical frequency was 50 h"1 and 45 h-1 for TC and DXC, respectively. The results obtained by the proposed method were in good agreement with those obtained by the official method at 95% confidence level.

A construção, avaliação e aplicação analítica de um sensor potenciométrico do tipo Pt|Hg|Hg2(Fur)2|Grafite, onde Fur significa íon 4-cloro-N-furfuril-5-sulfamoil-antranilato, são descritas. O eletrodo responde a Fur com sensibilidade de (-58,4 ± 0,9) mV década-1 no intervalo de 5,0 × 10-7-1,0 × 10-2 mol L-1, a pH 7,0-9,0 e com um limite de detecção de 3,8 × 10-7 mol L-1. O eletrodo é facilmente construído e de baixo custo, apresenta um rápido tempo de resposta (10-20 s) e pode ser usado por um período de 6 meses sem qualquer variação considerável nas suas características de desempenho. O eletrodo proposto mostrou boa seletividade na presença de várias substâncias, bem como na presença de alguns carboxilatos e ânions inorgânicos. O eletrodo foi aplicado com sucesso na determinação de furosemida em medicamentos, urina, soro sanguíneo e amostras comerciais de leite bovino.

The construction, evaluation and analytical application of a potentiometric sensor, namely, Pt|Hg|Hg2(Fur)2|Graphite, where Fur stands for 4-chloro-N-furfuryl-5-sulphamoyl-anthranilate ion, are described. This electrode has a linear dynamic range between 5.0 × 10-7-1.0 × 10-2 mol L-1 with a near-Nernstian slope of (-58.4± 0.9) mV decade-1 and a detection limit of 3.8 × 10-7 mol L-1. The potentiometric response is independent of the pH of the solution in the pH range 7.0-9.0. The electrode shows easy construction, low-cost, fast response time (within 10-20 s) and can be used for a period of 6 months without significant change in its performance characteristics. The proposed sensor displayed good selectivities over a variety of other anions (carboxylates and inorganic anions). Application of this potentiometric sensor for the furosemide determination in pharmaceuticals, urine, blood serum and commercial milk samples is reported.

No presente trabalho foi investigado o desenvolvimento de um método espectrofotométrico limpo para a determinação de formaldeído em amostras comerciais. A substituição de reagentes altamente perigosos foi explorada, de modo a atender aos princípios estabelecidos pela química verde. O método proposto baseou-se na reação entre formaldeído e ácido cromotrópico na presença de sulfato de magnésio, produzindo um complexo estável Mg2+/ciclotetracromotropileno (λmax = 535 nm). Não há relatos na literatura sobre a utilização da reação supramencionada na determinação de formaldeído. As condições experimentais foram otimizadas, aplicando-se a metodologia de superfície de resposta. A lei de Lambert-Beer é obedecida na faixa de concentração de 3 a 11 mg L-1 de formaldeído, com coeficiente de correlação de 0,999. O método proposto para a determinação de formaldeído foi aplicado em amostras comerciais de desinfetantes e defrizantes capilares. Os resultados compararam-se favoravelmente aos obtidos pelo método oficial, demonstrando exatidão e precisão satisfatórias.

A green spectrophotometric analytical method for determination of formaldehyde in commercial samples was designed and investigated. Replacement of hazardous reagents was explored to attain the clean chemistry standards. The method is based on formaldehyde reaction with chromotropic acid in the presence of magnesium sulphate producing a stable complex Mg2+/ cyclotetrachromotropylene (λmax = 535 nm). To the best of our knowledge, there are no reports on the use of the above mentioned reaction for this determination. The experimental conditions were optimized by the response surface methodologies. Beer's Law is obeyed in a concentration range of 3 to 11 mg L-1 of formaldehyde with a correlation coefficient of 0.999. The proposed method was applied for the determination of formaldehyde in commercial disinfectants and deffrizing hair products. The results were favorably compared with those of the official method, with good accuracy and precision.

Este artigo descreve um método simples, portátil e ambientalmente amigável para a rápida determinação de dipirona em medicamentos empregando a espectroscopia de reflectância difusa. O método proposto está baseado nas medidas de reflectância do composto alaranjado produzido na reação de spot-test entre dipirona e p-dimetilaminocinamaldeído (p-DAC), em meio ácido, usando papel de filtro como suporte sólido. Metodologias de planejamento de experimentos foram utilizadas para a otimização das condições experimentais. Todas as medidas de reflectância foram efetuadas em 510 nm e o intervalo linear foi de 1,42 <FONT FACE=Symbol>´</FONT> 10-4-2,85 <FONT FACE=Symbol>´</FONT> 10-3 mol L-1, com coeficiente de correlação de 0,999. Os limites de detecção (LOD) e de quantificação (LOQ) foram de 1,20 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1 e 4,00 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1, respectivamente. A precisão intradia e interdia foi avaliada na análise de uma solução de dipirona 7,90 <FONT FACE=Symbol>´</FONT> 10-4 mol L-1 (n = 10). Os coeficientes de variação foram 1,1 e 0,9%, respectivamente. O método proposto foi aplicado com êxito na determinação de dipirona em amostras comerciais de medicamentos. Não foram observadas interferências dos excipientes comuns em formulações farmacêuticas. Os resultados obtidos pelo método proposto estão em boa concordância com aqueles obtidos pelo procedimento da Farmacopéia Brasileira num nível de confiança de 95%.

This paper describes a simple, portable and environmentally friendly method for the rapid determination of dipyrone in pharmaceuticals by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound produced from the spot test reaction between dipyrone and p-dimethylaminocinnamaldehyde (p-DAC), in acid medium, using a filter paper as solid support. Experimental design methodologies were used to optimize the measurement conditions. All reflectance measurements were carried out at 510 nm and the linear range was from 1.42 <FONT FACE=Symbol>´</FONT> 10-4-2.85 <FONT FACE=Symbol>´</FONT> 10-3 mol L-1, with a correlation coefficient of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.20 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1 and 4.00 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1, respectively. The intraday precision and interday precision were studied for 10 replicate analyses of 7.90 <FONT FACE=Symbol>´</FONT> 10-4 mol L-1 dipyrone solution. The coefficients of variation were 1.1 and 0.9%, respectively. The proposed method was applied successfully to the determination of dipyrone in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level.

As características, o desempenho e a aplicação de um eletrodo do tipo Pt|Hg|Hg2(NAP)2|Graphite, onde NAP=íon naproxenato, são descritas. O eletrodo responde a NAP com sensibilidade de (58,1± 0,9) mV década-1 no intervalo de 5,0 x 10-5 - 1,0 x 10-2 mol L-1 , a pH 6,0-9,0 e com um limite de detecção de 3,9 x 10-5 mol L-1. O eletrodo é de baixo custo e facilmente construído, apresenta um rápido tempo de resposta (10-35 s) e pode ser usado por um período de seis meses sem qualquer divergência considerável nos potenciais. O sensor supracitado mostrou boa seletividade para naproxeno na presença de várias substâncias, tais como carboxilatos e ânions inorgânicos, sendo aplicado na análise direta de naproxeno em medicamentos (comprimidos) via método da adição de padrão. Os resultados analíticos obtidos com o eletrodo proposto estão em boa concordância com aqueles obtidos pelo procedimento preconizado na Farmacopéia Americana.

The characteristics, performance, and application of an electrode, namely, Pt|Hg|Hg2(NAP)2|Graphite, where NAP stands for naproxenate ion, are described. This electrode responds to NAP with sensivity of (58.1± 0.9) mV decade-1 over the range 5.0 x 10-5 - 1.0 x 10-2 mol L-1 at pH 6.0-9.0 and a detection limit of 3.9 x 10-5 mol L-1. The electrode is easily constructed at a relatively low cost with fast response time (within 10-35 s) and can be used for a period of 6 months without any considerable divergence in potentials. The proposed sensor displayed good selectivity for naproxen in the presence of several substances, especially concerning carboxylate and inorganic anions. It was used for the direct assay of naproxen in commercial tablets by means of the standard additions method. The analytical results obtained by using this electrode are in good agreement with those given by the United States Pharmacopeia procedure.

Este trabalho descreve um método simples e rápido por "spot test" quantitativo, utilizando a espectroscopia de reflectância difusa para determinação de metildopa em formulações farmacêuticas. O método proposto baseia-se na reação de complexação entre metildopa e íons molibdato, formando um complexo amarelo na superfície do papel de filtro. As medidas de reflectância foram realizadas a 410 nm. A curva analítica obtida a partir do gráfico de densidade óptica do sinal de reflectância (A R) vs. log da concentração de metildopa apresentou linearidade na faixa de 6,30 x 10-3 a 1,89 x 10-2 mol L-1, com um coeficiente de correlação de 0,998. O limite de detecção foi de 2,74 x 10-3 mol L-1 (R.S.D. = 1,02%). As substâncias comumente utilizadas como excipientes nas formulações farmacêuticas não interferem no método proposto. O método foi aplicado para a determinação de metildopa em formulações farmacêuticas comerciais. Os resultados obtidos por este método foram comparados favoravelmente com aqueles obtidos pelo método oficial, com 95% de nível de confiança.

This paper describes a very simple and rapid quantitative reflectance spot test procedure for the determination of methyldopa in pharmaceutical formulations. This method is based on the complexation reaction of methyldopa with molybdate ions yielding a yellow stable complex on filter paper. Reflectance measurements were carried out at 410 nm. Under optimal conditions, the calibration graphs obtained for methyldopa by plotting the optical density of the reflectance signal (A R) vs. the log of the concentration were linear from 6.30 x 10-3 to 1.89 x 10-2 mol L-1, with a correlation coefficient of 0.998. The detection limit was 2.74 x 10-3 mol L-1 (R.S.D. = 1.02%) for methyldopa. The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine metyldopa in commercial pharmaceutical formulations. The results obtained by the proposed method compare favorably with those obtained by an official procedure at 95% confidence level.