Resumo em Inglês:

The physicochemical properties of 2,4-, and 3,4- dimethoxybenzoates of Cu(II), Co(II) and Nd(III) were studied and compared to observe the -OCH3 substituent positions in benzene ring on the character of complexes. The analysed compounds are crystalline hydrated or anhydrous salts with colours depending on the kind of central ions: blue for Cu(II), pink for Co(II) and violet for Nd(III) complexes. The carboxylate groups bind as monodentate, bidentate bridging or chelating and even tridentate ligands. Their thermal stabilities were studied in air at 293-1173K. When heated the hydrated complexes release the water molecules and form anhydrous compounds which are then decomposed to the oxides of respective metals. Their magnetic moment values were determined in the range of 76-303K. The results reveal the compounds of Nd(III) and Co(II) to be the high-spin and that of Cu(II) forms dimer. The various positions of -OCH3 groups in benzene ring influence some of physicochemical properties of analysed compounds.

Resumo em Inglês:

A new Cu(II) trimers, [Cu3(dcp)2(H2O)8]. 4DMF, with the ligand 3,5-pyrazoledicarboxylic acid monohydrate (H3dcp) has been prepared by solvent method. Its solid-state structure has been characterized by elemental analysis, thermal analysis (TGA and DSC), and single crystal X-ray diffraction. X-ray crystallographic studies reveal that this complex has extended 1-D,2-D and 3-D supramolecular architectures directed by weak interactions (hydrogen bond and aromatic π-π stacking interaction) leading to a sandwich solid-state structure.

Resumo em Inglês:

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves the reduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer's law for 0.6-7.5 and 0.5-5.0 µg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 10(4) and 1.06 X 10(5) Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039µg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student's t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.

Resumo em Inglês:

Voltammetric technique was used to study the binary and ternary complexes of cadmium with L-amino acids and vitamin-C (L-ascorbic acid) at pH =7.30 ± 0.01, µ = 1.0M KNO3 at 25ºC and 35ºC. Cd (II) formed 1:1:1, 1:1:2 and 1:2:1 complexes with L-lysine, L-ornithine, L-threonine, L-serine, L-phenylglycine, L-phenylalanine, L-glutamic acid and L-aspartic acid used as primary ligands and L-ascorbic acid used as secondary ligand. The trend of stability constant of complexes was L-lysine < L-ornithine < L-threonine < L-serine < L-phenylglycine < L-phenylalanine < L-glutamic acid < L-aspartic acid which can be explained on the basis of size, basicity and steric hindrance of ligands. The values of stability constant (log β) varied from 2.23 to11.33 confirm that these drugs i.e. L-amino acids or in combination with L-ascorbic acid or their complexes could be used against Cd (II) toxicity. The study has been carried out at 35ºC also to determine the thermodynamic parameters such as enthalpy change (ΔH), Free energy change (ΔG) and entropy change (ΔS) respectively.

Resumo em Inglês:

A direct, extraction-free spectrophotometric method has been developed for the determination of acebutolol hydrochloride (ABH) in pharmaceutical preparations. The method is based on ion-pair complex formation between the drug and two acidic dyes (sulphonaphthalein) namely bromocresol green (BCG) and bromothymol blue (BTB). Conformity to Beer's law enabled the assay of the drug in the range of 0.5-13.8 µg mL-1 with BCG and 1.8-15.9 µg mL-1 with BTB. Compared with a reference method, the results obtained were of equal accuracy and precision. In addition, these methods were also found to be specific for the analysis of acebutolol hydrochloride in the presence of excipients, which are co-formulated in the drug.

Resumo em Inglês:

A simple spectrophotometric method for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin with variamine blue is presented. The determination is based on the hydrolysis of β-lactam ring of cephalosporins with sodium hydroxide which subsequently reacts with iodate to liberate iodine in acidic medium. The liberated iodine oxidizes variamine blue to violet colored species of maximum absorption at 556 nm. The absorbance is measured within the pH range of 4.0-4.2. Beer's law is obeyed in the range of 0.5-5.8 µg mL-1, 0.2-7.0 µg mL-1, 0.2-5.0 µg mL-1 and 0.5-8.5 µg mL-1 for cefotaxime, ceftriaxone, cefadroxil and cephalexin respectively. The analytical parameters were optimized and the method is successfully applied for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin in pharmaceuticals.

Resumo em Português:

Um procedimento de injeção em fluxo com detecção espectrofotométrica para a determinação de paracetamol foi descrito. O procedimento foi baseado na reação de oxidação do paracetamol pelo hipoclorito de sódio e a determinação de seu excesso empregando o dicloreto de o-tolidina como reagente cromogênico. A curva analítica apresentou um comportamento linear entre as concentrações de paracetamol de 8,5 x 10-6 a 2,51 x 10-4 mol L-1 com um limite de detecção de 5,0 x 10-6 mol L-1. O desvio padrão relativo foi menor que 1,2% para uma solução de paracetamol de 1,20 x 10-4 mol L-1 (n=10). Os resultados obtidos nas análises de produtos farmacêuticos comerciais obtidos empregando o procedimento desenvolvido foram comparados com aqueles obtidos empregando o procedimento descrito na Farmacopéia Americana (USP XXII) estando em concordância ao nível de confiança de 95%.

Resumo em Inglês:

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

Resumo em Português:

Uma das cargas mais utilizadas na fabricação de espumas flexíveis de poliuretano é o carbonato de cálcio (CaCO3) por ser não abrasivo, não tóxico e de fácil pigmentação. Contudo, é observado que o excesso de CaCO3 comercial usado nas indústrias causa deformações permanentes, o que prejudica a qualidade do produto final. No presente trabalho é proposto o estudo do efeito da concentração de CaCO3 comercial na fabricação de espumas flexíveis de poliuretano. Foram utilizadas diferentes concentrações de CaCO3 na síntese das espumas, as quais foram submetidas à análises térmica e morfológica, afim de verificar as alterações provocadas pela introdução progressiva da carga.

Resumo em Inglês:

One filler often utilized in flexible polyurethane foams is calcium carbonate (CaCO3) because it is non-abrasiveness, non-toxicity and facilitated pigmentation. However, it is observed that the excess of commercial CaCO3 utilized in industry possibly causing permanent deformations and damaging the quality of the final product. The effect of different concentrations of commercial CaCO3, in flexible foams, was studied. Different concentrations of CaCO3 were used for the synthesis of flexible polyurethane foams, which were submitted to morphological and thermal analyses to verify the alterations provoked by the progressive introduction of this filler.

Resumo em Inglês:

A procedure for separation and preconcentration of trace amounts of Zn(II) from aqueous media is proposed. The procedure is based on the adsorption of Zn2+ on octadecyl bonded silica membrane disk modified with N,N'-disalicylidene-1,2-phenylendiamine at pH 7. The retained zinc ions were then stripped from the disk with a minimal amount of 1.5 mol L-1 hydrochloric acid solution as eluent, and determined by flame atomic absorption spectrometry. Maximum capacity of the membrane disk modified with 5 mg of the ligand was found to be 226 µg Zn2+. The relative standard deviation of zinc for ten replicate extraction of 10 µg zinc from 1000 mL samples was 1.2%. The limit of detection of the proposed method was 14 ng of Zn2+ per 1000 mL. The method was successfully applied to the determination of zinc in natural water samples and accuracy was examined by recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry (GFAAS).

Resumo em Português:

Este trabalho apresenta um método de análise por injeção em fluxo para determinação quantitativa de cloridrato de vancomicina, C66H75Cl2N9O24.HCl (HVCM), baseado na reação com íons cobre (II). ? HVCM na presença de íons cobre, em pH≅4,5 e solução aquosa forma um complexo azullilás, com absorção máxima em 555 nm. O limite de detecção estimado foi de 8.5×10-5 mol L-1; e o limite de quantificação de 2.5×10-4 mol L-1 com cerca de 30 determinações por hora. A exatidão do método foi determinada através de ensaio de recuperação na presença de quatro diferentes excipientes na proporção de 1:1 p/p. Os resultados do método espectrofotométrico por injeção em fluxo foram comparados com resultados obtidos pelo método espectrofotométrico por batelada e por HPLC, através de método estatístico t de Student. Obteve-se completa concordância com nível de significância de 0,95 e similar precisão (RSD: 2,1 % vs. 1,9%).

Resumo em Inglês:

A flow injection method for the quantitative analysis of vancomycin hydrochloride, C66H75Cl2N9O24.HCl (HVCM), based on the reaction with copper (II) ions, is presented. HVCM forms a lilac-blue complex with copper ions at pH≅4.5 in aqueous solutions, with maximum absorption at 555 nm. The detection limit was estimated to be about 8.5×10-5 mol L-1; the quantitation limit is about 2.5×10-4 mol L-1 and about 30 determinations can be performed in an hour. The accuracy of the method was tested through recovery procedures in presence of four different excipients, in the proportion 1:1 w/w. The results were compared with those obtained with the batch spectrophotometric and with the HPLC methods. Statistical comparison was done using the Student's procedure. Complete agreement was found at a 0.95 significance level between the proposed flow injection and the batch spectrophotometric methods, which present similar precision (RSD: 2.1 % vs. 1.9%).