Content uniformity (CU) is a parameter used to ensure the uniformity of the amount of active substances in pharmaceutical preparations. It is often evaluated in the quality control of pharmaceutical dosage forms, and a novel method was proposed for CU determination using thermal infrared enthalpimetry (TIE). Captopril tablets were dissolved in 24-well microplates and the heat released from the reaction of captopril and I2 was monitored with an infrared camera. Some experimental parameters were adjusted, as captopril/I2 ratio, stirring speed and dispensing rate, and the most suitable conditions were 1.00:1.00 (v/v), 250 rpm and 0.57 mL s-1, respectively. Interferences from tablet adjuvants (e.g., starch, cellulose and lactose) were not observed. The results obtained by TIE did not differ statistically (Student’s t-test, p > 0.05) from those from official method (UV spectrophotometry) described in pharmacopeia. The TIE method required 31 and 12 times less reagent and time, respectively. Therefore, the proposed method was suitable for routine analysis and agrees with the requirements of green analytical chemistry.

PdCl2 immobilized in polyacrylamide (PAM), named Pd/PAM, produced at an extremely low cost, was found to be an efficient catalyst for Suzuki-Miyaura cross-coupling reactions. Iodo- and bromoarenes may couple with phenylboronic acid under eco-friendly conditions (i.e., phosphine-free and with ethanol as the solvent) to give excellent product yields. Aryl chlorides, in contrast, were found to be unsuitable reagents in this context, yielding modest results. The recyclability of Pd/PAM is limited because of PdII leaching, which leaves only the base polymer on the surface after six runs. The Pd/PAM catalyst was initially prepared via the formation of a PAM hydrogel using an aqueous PdCl2 solution. After drying, the solid Pd/PAM was characterized by scanning electron microscopy (SEM), electron-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), and inductively coupled plasma optical emission spectrometry (ICP OES).

We herein described the preparation of a novel series of limonin derivatives (modification in A-ring), which was synthesized efficiently using methodology in solution as well as in heterogeneous medium (K-10). In addition, we obtained derivatives by inserting the 1,2,3-triazole nucleus via click reaction and also prepared derivatives from reactions with limonin-7-oxime. All compounds were submitted to investigation of the antimicrobial activity against a collection of microorganisms. The results of the antimicrobial activity, in general, demonstrated that a relevant number of synthetic derivatives presented higher activity than the natural product.

Elementos traço e majoritários foram determinados em mexilhão dourado (Limnoperna fortunei) coletados no canal São Gonçalo (Rio Grande-RS, Brasil). Digestão assistida por microondas em sistema fechado foi utilizada para decomposição das amostras com subsequente determinação elementar por técnicas espectrométricas. Os resultados mostraram que o tecido de mexilhão contém Ag, Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, Li, Mg, Mn, Mo, P, Pb, S, Sn, Sr, Ti, V e Zn, enquanto que na casca foram encontrados os mesmo elementos, exceto Ag e Hg, evidenciando seu potencial como biomarcador. Neste sentido, estes resultados podem ser utilizados para estabelecer um panorama inicial e contribuir para futuros estudos relacionados a contaminantes inorgânicos na área estudada.

Major and trace element content was determined in golden mussel (Limnoperna fortunei) collected in the São Gonçalo Channel (Rio Grande City, Brazil). A microwave-assisted digestion procedure in closed vessels was applied to mussel decomposition and subsequent determination of elements by spectrometric techniques. Results showed that the mussel tissue contains Ag, Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, Li, Mg, Mn, Mo, P, Pb, S, Sn, Sr, Ti, V and Zn, while the same elements (except Ag and Hg) were quantified in its shell, demonstrating its potential as a biomarker. In this sense, these results can be used to establish an initial view and to contribute to further studies related to element contamination in the area under study.

Neste trabalho foi utilizada a piroidrólise para a decomposição de suplemento mineral utilizado na nutrição animal, para a posterior determinação de F, Br e I. Flúor foi determinado por potenciometria utilizando eletrodo íon-seletivo para fluoreto, enquanto que Br e I foram determinados por espectrometria de massa com plasma indutivamente acoplado. Os principais parâmetros que influenciam a piroidrólise foram investigados e, após a devida avaliação dos mesmos, foram fixadas as seguintes condições: a temperatura do reator em 1000 °C durante 10 min; a proporção entre a massa de amostra e a massa de acelerador em 1 + 5 e a vazão do gás carreador em 200 mL min-1. A exatidão do método foi avaliada usando teste de recuperação do analito e análise de materiais de referência certificados de rocha fosfática e de solo. O método foi aplicado para análise de suplemento mineral. Os limites de quantificação foram de 16, 0,3 e 0,07 µg g-1 para F, Br e I, respectivamente. Assim, usando-se um método relativamente simples e de baixo custo é possível a decomposição de até 5 amostras por hora. Portanto, a piroidrólise pode ser usada como um método de rotina para o preparo de amostra de suplemento mineral para a determinação de F, Br e I.

Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 ºC during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min-1. The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 µg g-1 for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements.

O sistema de degradação utilizando ferro metálico e peróxido de hidrogênio (reação de Fenton) foi empregado para a degradação do herbicida diurom. Visando obter as melhores condições de degradação, foram otimizados parâmetros que influenciam no processo, como pH, concentração de peróxido de hidrogênio (H2O2) e quantidade de ferro. A degradação do herbicida foi acompanhada por cromatografia líquida com detecção por arranjo de diodos (CLAE-DAD) e cromatografia líquida com detecção por espectrometria de massas sequencial (LC-ESI-MS/MS), além da determinação de carbono orgânico total (COT). Nas melhores condições de degradação, pH = 2,5; 2 g de ferro e 2 mmol L-1 de H2O2, uma solução aquosa de diurom comercial (10 mg L-1), alcançou valores não detectáveis ao tempo de 10 min, para diurom e para o metabólito monitorado, 3,4-DCA. Ainda os valores de COT foram reduzidos, chegando a valores menores que 5 mg L-1, mostrando a eficiência e rapidez do sistema.

A degradation system using metallic iron and hydrogen peroxide (Fenton reaction) was employed for the degradation of the diuron herbicide. In order to obtain the maximum degradation the main conditions such as pH, hydrogen peroxide concentration and iron amount, were optimized. Herbicide degradation was evaluated by liquid chromatography with diode array detection (HPLC-DAD) and liquid chromatography tandem mass spectrometric detection (LC-ESI-MS/MS) and total organic carbon analysis (TOC). In the best degradation condition, pH = 2.5, 2 g of iron and 2 mmol L-1 of hydrogen peroxide, after 10 min a commercial diuron solution (10 mg L-1) had no detection values for diuron and its metabolic, 3,4-dichloroaniline (3,4-DCA). The TOC was reduced to values lower than 5 mg L-1 showing the efficiency of the system.

Pyrohydrolysis is proposed for fossil fuels sample preparation for further fluorine and chlorine determination. Samples were heated during 10 min at temperatures up to 1000 °C. Water vapor was passed through the reactor and the volatile products were condensed and collected in NH4OH solution. Fluoride was determined by potentiometry using an ion selective electrode (ISE) and Cl by ICP OES and DRC-ICP-MS. The results are in good agreement with certified values and the precision is better than 10% (n = 4). Sample preparation by means of pyrohydrolysis is relatively simple, whereas chlorine and fluorine can be determined at low concentrations.