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Journal of Thermal Analysis and Calorimetry
Authors: Lakshmi Kaza, Hany F. Sobhi, Jeffrey A. Fruscella, Chris Kaul, Shravan Thakur, Naullage I. Perera, Kenneth Alexander, and Alan T. Riga

Abstract

A standard protocol was developed to determine the water content by thermal analysis of milk of magnesia (MoM). Differential scanning calorimetry (DSC) and thermogravimetry (TG) were used in a novel manner for examining the physical characteristics of the commercial pharmaceutical suspensions. Moisture analyzer and oven-dry methods validate the proposed protocol. MoM consists primarily of water and magnesium hydroxide [Mg(OH)2]. Experimental design of the thermal analysis parameters were considered including sample size, flowing atmosphere, sample pan, and heating rate for both DSC and TG. The results established the optimum conditions for minimizing heat and mass transfer effect. Sample sizes used were: (5–15 mg) for DSC and (30–50 mg) for TG. DSC analysis used crimped crucibles with a pinhole, which allowed maximum resolution and gave well-defined mass (water) loss. TG analysis used a heating rate of 10 °C/min−1 in an atmosphere of nitrogen. The heat of crystallization, heat of fusion, and heat of vaporization of unbound water are 334, 334, and 2,257 Jg−1, respectively (Mitra et al. Proc NATAS Annu Conf Therm Anal Appl 30:203–208, ). The DSC average water content of (MoM) was 80 wt% for name brand and 89.5 wt% for generic brand, based on the relative crystallization, melting and vaporization heats/Jg−1 of distilled water in the recently purchased (2011) MoM samples. The TG showed a two-step process, losing water at 80–135 °C for unbound water and bound water (MgO·H2O) at 376–404 °C, yielding a total average water loss of 91.9 % for name brand and 90.7 % for generic brand by mass. The difference between the high-temperature TG and the lower-temperature DSC can be attributed for the decomposition of magnesium hydroxide or MgO·H2O. Therefore in performing this new approach to water analysis by heating to a high temperature decomposed the magnesium hydroxide residue. It was determined that the TG method was the most accurate for determining bound and unbound water.

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Journal of Thermal Analysis and Calorimetry
Authors: Libby Yoerg, M. Ellen Matthews, Lakshmi Kaza, Naullage Indika Perera, David W. Ball, John Moran, and Alan T. Riga

Abstract

Three aldohexose monosaccharides, d-glucose, d-mannose, and d-galactose, were examined by scanning temperature dielectric analysis (DEA) from ambient temperatures through their melts. Phase transitions, including glass transition (Tg) and melting temperature (Tm), were evaluated by differential scanning calorimetry (DSC). The monosaccharides were found to exhibit thermally-induced dielectric loss spectra in their amorphous-solid phase before melting. Activation energies for electrical charging of each of the monosaccharides were calculated from an Arrhenius plot of the tan delta (e″/e′, dielectric loss factor/relative permittivity) peak frequency versus reciprocal temperature in Kelvin. The DEA profiles were also correlated with the DSC phase diagrams, showing the changes in electrical behavior associated with solid–solid and solid–liquid transitions.

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Solid-state mechanical properties of crystalline drugs and excipients

New data substantiate discovered dielectric viscoelastic characteristics

Journal of Thermal Analysis and Calorimetry
Authors: Shravan Singh Thakur, Manik Pavan Kumar Maheswaram, Dhruthiman Reddy Mantheni, Lakshmi Kaza, Indika Perara, David W. Ball, John Moran, and Alan T. Riga

Abstract

Thermal mechanical analysis (TMA) of crystalline drugs and excipients in their pre-melt temperature range performed in this study corroborate their newly found linear dielectric conductivity properties with temperature. TMA of crystalline active pharmacy ingredients (APIs) or excipients shows softening at 30–100 °C below the calorimetric melting phase transition, which is also observed by dielectric analysis (DEA). Acetophenetidin melts at 135 °C as measured calorimetrically by DSC, but softens under a low mechanical stress at 95 °C. At this pre-melting temperature, the crystals collapse under the applied load, and the TMA probe shows rapid displacement. The mechanical properties yield a softening structure and cause a dimensionally slow disintegration resulting in a sharp dimensional change at the melting point. In order to incorporate these findings into a structure–property relationship, several United States Pharmacopeia (USP) melting-point standard drugs were evaluated by TMA, DSC, and DEA, and compared to the USP standard melt temperatures. The USP standard melt temperature for vanillin (80 °C) [], acetophenetidin (135 °C) [], and caffeine (235 °C) [] are easily verified calorimetrically via DSC. The combined thermal analysis techniques allow for a wide variety of the newly discovered physical properties of drugs and excipients.

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