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.
Authors:R. Macêdo, O. de Moura, A. de Souza, and A. Macêdo
This work present comparative results on powder milk storage quality, obtained from analytical methods. Protein content was
determined conventional (Kjeldahl) and colorimetric with biuret reagent at 540 nm and integral quality by thermogravimetric
and biological methods. A method was developed for the protein separation of powder milk. Powder milk was submitted to degradation
processes at 45, 60 and 80°C for 20 days. The results indicated that protein content values were inconsistent if determinations
by Kjeldahl and colorimetric methods and biological tests were compared. There is evidence of thermal decomposition of powder
milk as detected by biological and thermogravimetric methods.
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
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.
Authors:Ana Gomes, Lidiane Correia, Mônica da Silva Simões, and R. Macêdo
The objective of this work was to develop
and validate a fast and reproducible method to determine the concentration
of metronidazole in drug substance and tablets. The samples were analyzed
by dynamic thermogravimetry, using 10, 20, 40, 60 and 80C min–1
heating rates in nitrogen and in nitrogen with synthetic air. Obtained data
were used in the Antoine and Langmuir equations in order to have the pressure
curves. Vapor pressure curves of drug and tablet of metronidazole were evaluated
using the mathematical indexes of difference factor, f1,
and similarity factor, f2,
to compare their profiles. The data showed that there is no significant difference
between the vapor pressure profiles of drug and tablet of metronidazole in
both environmental conditions, which confirms that the process is really vaporization.
The concentration of metronidazole was determined in the raw material and
tablets of the drug.
Authors:F. Santos de Souza, A. Gomes Barreto, and R. Macêdo
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.
Authors:A. de Medeiros, N. de Cervantes, A. Gomes, and R. Macêdo
TG and DSC data were used to determine the thermal parameters of prednisone drug and tablets. Two formulations of prednisone
20 mg were analysed in the form of tablets. The TG curves of prednisone drug and tablets A and B displayed six, eight and
seven thermal decomposition processes, respectively. Analysis of the DSC data pointed to chemical interactions between prednisone
drug and the excipients of tablets A and B, suggested by alterations in the melting temperature of prednisone. The analysis
revealed that prednisone drug is more stable than tablets A and B.
Authors:Ana Medeiros, Lidiane Correia, Mônica Simões, and R. Macêdo
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