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Abstract  

This work proposes thermal characterization as analytical methodology for the identification and purity assay of warifteine, an alkaloid in Cissampelos sympodialis Eichl. Thermal and kinetic parameters were determined by means of TG and DSC photovisual studies. The TG results showed that the decomposition of warifteine in air and nitrogen atmospheres proceeds in three and four steps, respectively. The TG data allowed calculation of the kinetic parameters of warifteine. The activation energy values obtained by different methods displayed a good correlation. With the DSC photovisual system applied it is possible to detect the impurity level in warifteine after its purification.

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Journal of Thermal Analysis and Calorimetry
Authors: Rosali Ferreira da Silva, Flávia Morais de Medeiros, T. Nascimento, R. Macêdo, and P. Neto

Abstract  

The object of the present work is to study the thermal characteristics of indinavir sulfate and to evaluate the quality of the raw materials. Indinavir A, B, C and reference samples were obtained from different suppliers and submitted to TG, DSC and DSC-photovisual analyses. TG/DTG curves indicated a desolvation and dehydration processes and were confirmed by DSC. According to the DSC curves the fusion took place at about 141–142°C for indinavir C and Reference sample B and about 146–149°C for the others. DSC-photovisual showed insoluble raw materials for indinavir C at 160°C. Indinavir sulfate is highly hygroscopic drug which requires attention during storage and manufacture by pharmaceutical industry.

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Abstract  

This study demonstrates the thermalanalysis applications in compatibility and stability studies of the propranolol binary mixture sand tablets A and B. The propranolol binary mixtures were prepared in the laboratory and compared to the fully formulated tablets using the thermogravimetric (TG) and calorimetric(DSC) methods. DSC of binary mixtures showed similar phase transition to propranolol drug. The tablets phase transition decreased and there was no detectable significant interaction in propranolol–lactose mixture and tablets. The DSC-photovisual test revealed an interaction similar to the Maillard reaction. The TG isothermal study showed a difference in the profile between the drug and tablets due excipients quality and problems in manufacture process. The kinetic parameters indicated a lower stability for the tablets than propranolol drug. The thermal techniques thermally differentiated the propranolol preparations demonstrating the importance in the design development of pharmaceuticals solid-dosage form.

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Abstract  

A number of disintegrants are available on the market. They improve tablets’ disintegration. The objective of this work is the comparison of the technological quality parameters of disintegrants using different analytical techniques. Three batches of disintegrants and their binary mixtures (water:disintegrants) were investigated. Cooling experiments were used from –30 up to 200C. The data obtained showed calorimetric differences between the samples. In the binary mixtures water showed different crystallization behaviour from the one found in the literature. According to the results DSC technique helped the quality control of different disintegrants.

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Journal of Thermal Analysis and Calorimetry
Authors: Agna Hélia de Oliveira, Elisana Afonso de Moura, Márcia Ferraz Pinto, José Valdilânio Virgulino Procópio, Valmir Gomes de Souza, Fábio Santos de Souza, and Rui Oliveira Macêdo

(DSC), and Differential Scanning Calorimetry coupled to photovisual system (DSC photovisual)] and Pyrolysis coupled to Gas chromatography/Mass spectrometry (Pyr-GC/MS). Experimental Samples Sample of

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Abstract  

This article had studied the thermal characterization of the raw material and different fluconazole crystals, obtained through recrystallization with different solvents using thermoanalytical techniques (TG, DTA, DSC-50, DSC Photovisual, DSC-60) and Pyr-GC/MS. The results confirmed that the fluconazole volatilizes without decomposition until 250 °C. Pyr-GC/MS showed hexachlorobenzene like impurities in fluconazole raw material.

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Abstract  

Thermal characterization is proposed as analytical methodology for the purity assay of lapachol, and for determination of the quality parameters of capsules containing this molecule. The TG data revealed that lapachol is more stable in the presence of adjuvants, showing the good quality of the formulation. The kinetic parameters obtained were lower for lapachol drug than for the formulated lapachol. The DSC data demonstrated good compatibility between lapachol drug and the adjuvant in the formulated lapachol, and did not reveal impurities such as secondary products of the isolation and recrystallization processes. The data were confirmed by the DSC-photovisual findings.

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Abstract  

The present work proposes evaluation of the gelatinization processes of starch by means of DSC coupled with a photovisual system. The use of DSC, TG and DTA for a fast and efficient evaluation of the starch is suggested. The DSC curves of starch gels with water contents of 20, 30, 40 and 50% (mass/v) exhibited different phase transitions, corresponding to the gelatinization processes at the different water contents for the different lots. The DSC-photovisual system confirmed calorimetric behaviour differences between the starch lots studied.

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Journal of Thermal Analysis and Calorimetry
Authors: Antonilêni Medeiros, Ana Santos, F. de Souza, J. Procópio, Márcia Pinto, and R. Macêdo

Abstract  

Stability of drugs and products has a great practical interest, which is facing to strict regulation. Thermal studies, besides the determination of the thermal properties of the investigated product allow the verification of possible interactions between the drug substances and excipients. The objective of this work was to obtain solid pre-formulates of paracetamol (PC) by spray drying (SPDR), as well as to investigate their thermal behavior. Dynamic and isotherm TG, conventional DSC and DSC-photovisual coupled methods were used to characterize the conventional and pre-formulated mixtures obtained by SPDR. The results of both DSC investigations showed slight alterations in melting temperatures, which suggests incompatibilities. The TG decomposition data of the mixtures evidenced that the dry process via SPDR leads to stability enhancement of the pre-formulated mixtures.

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Abstract  

The compatibilities and stabilities of some binary mixtures and generic hydrochlorothiazide formulations were studied by using TG, DSC and a DSC-photovisual system. The kinetic parameters were determined via the Arrhenius equations. Tablet B presented higher compatibility and thermal stability than those of tablets A and C. The photovisual system demonstrated that the decomposition of tablet A occurs before the melting point, due to the Maillard reaction between the hydrochlorothiazide and lactose present in the formulation. The behaviour and rate constants of binary mixtures suggest that lactose can be substituted for microcrystalline cellulose, MC(101), in tablet A. The DSC and TG data revealed different characteristics of compatibility and stability in generic formulations from different manufacturers.

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