1.In-depth investigation on physicochemical and thermal properties of magnesium (II) gluconate using spectroscopic and thermoanalytical techniques
Trivedi Kumar MAHENDRA ; Dixit NEENA ; Panda PARTHASARATHI ; Sethi Kumar KALYAN ; Jana SNEHASIS
Journal of Pharmaceutical Analysis 2017;7(5):332-337
Magnesium gluconate is a classical organometallic pharmaceutical compound used for the prevention and treatment of hypomagnesemia as a source of magnesium ion. The present research described the in-depth study on solid state properties viz. physicochemical and thermal properties of magnesium gluconate using sophisticated analytical techniques like Powder X-ray diffraction (PXRD), particle size analysis ( PSA), Fourier transform infrared (FT-IR) spectrometry, ultraviolet–visible (UV–Vis) spectroscopy, thermogravimetric analysis (TGA)/differential thermogravimetric analysis (DTG), and differential scanning calorimetry (DSC). Magnesium gluconate was found to be crystalline in nature along with the crystallite size ranging from 14.10 to 47.35 nm. The particle size distribution was at d(0.1)=6.552 μm, d(0.5)=38.299 μm, d(0.9)=173.712 μm and D(4,3)=67.122 μm along with the specific surface area of 0.372 m2/g. The wavelength for the maximum absorbance was at 198.0 nm. Magnesium gluconate exhibited 88.51% weight loss with three stages of thermal degradation process up to 895.18 ℃ from room temperature. The TGA/DTG thermograms of the analyte indicated that magnesium gluconate was thermally stable up to around 165 ℃. Consequently, the melting temperature of magnesium gluconate was found to be 169.90 ℃ along with the enthalpy of fusion of 308.7 J/g. Thus, the authors conclude that the achieved results from this study are very useful in pharmaceutical and nutraceutical industries for the identification, characterization and qualitative analysis of magnesium gluconate for preformulation studies and also for developing magnesium gluconate based novel formulation.
2.In-depth investigation on physicochemical and thermal properties of magnesium (II) gluconate using spectroscopic and thermoanalytical techniques
Trivedi Kumar MAHENDRA ; Dixit NEENA ; Panda PARTHASARATHI ; Sethi Kumar KALYAN ; Jana SNEHASIS
Journal of Pharmaceutical Analysis 2017;7(5):332-337
Magnesium gluconate is a classical organometallic pharmaceutical compound used for the prevention and treatment of hypomagnesemia as a source of magnesium ion. The present research described the in-depth study on solid state properties viz. physicochemical and thermal properties of magnesium gluconate using sophisticated analytical techniques like Powder X-ray diffraction (PXRD), particle size analysis ( PSA), Fourier transform infrared (FT-IR) spectrometry, ultraviolet–visible (UV–Vis) spectroscopy, thermogravimetric analysis (TGA)/differential thermogravimetric analysis (DTG), and differential scanning calorimetry (DSC). Magnesium gluconate was found to be crystalline in nature along with the crystallite size ranging from 14.10 to 47.35 nm. The particle size distribution was at d(0.1)=6.552 μm, d(0.5)=38.299 μm, d(0.9)=173.712 μm and D(4,3)=67.122 μm along with the specific surface area of 0.372 m2/g. The wavelength for the maximum absorbance was at 198.0 nm. Magnesium gluconate exhibited 88.51% weight loss with three stages of thermal degradation process up to 895.18 ℃ from room temperature. The TGA/DTG thermograms of the analyte indicated that magnesium gluconate was thermally stable up to around 165 ℃. Consequently, the melting temperature of magnesium gluconate was found to be 169.90 ℃ along with the enthalpy of fusion of 308.7 J/g. Thus, the authors conclude that the achieved results from this study are very useful in pharmaceutical and nutraceutical industries for the identification, characterization and qualitative analysis of magnesium gluconate for preformulation studies and also for developing magnesium gluconate based novel formulation.
3.Solid and liquid state characterization of tetrahydrocurcumin using XRPD, FT-IR, DSC, TGA, LC-MS, GC-MS, and NMR and its biological activities
Trivedi Kumar MAHENDRA ; Panda PARTHASARATHI ; Sethi Kumar KALYAN ; Gangwar MAYANK ; Mondal Charan SAMBHU ; Jana SNEHASIS
Journal of Pharmaceutical Analysis 2020;10(4):334-345
Tetrahydrocurcumin (THC) is one of the major metabolites of curcumin (CUR), an ancient bioactive natural polyphenolic compound. This research article describes both the solid and liquid state charac-terization of THC using advanced spectroscopic and thermo-analytical techniques. Anti-inflammatory, anti-oxidant, and neuroprotective activities of THC were investigated using in vitro cell lines. Liquid chromatography-mass spectrometry analysis revealed that our sample comprised 95.15% THC, 0.51% tetrahydrodemethoxycurcumin (THDC), 3.40% hexahydrocurcumin, and 0.94% octahydrocurcumin. Gas chromatography-mass spectrometry analysis indicated the presence of 96.68% THC and 3.32% THDC. THC in solution existed as keto-enol tautomers in three different forms at different retention time, but the enol form was found to be dominant, which was also supported by nuclear magnetic resonance analysis. THC was thermally stable up to 335.55 ℃. THC exhibited more suppression of cytokines (TNF-α, IL-1β, and MIP-1α) than CUR in a concentration-dependent manner in mouse splenocytes, while NK-cell and phagocytosis activity was increased in macrophages. THC showed a significant reduction of free radicals (LPO) along with improved antioxidant enzymes (SOD and catalase) and increased free radical scav-enging activity against ABTS+ radicals in HepG2 cells. THC displayed higher protection capability than CUR from oxidative stress and neuronal damage by improving cell viability against H2O2 induced HepG2 cells and MPP+ induced SH-SY5Y cells, respectively, in a concentration-dependent manner. Thus, a variation of the biological activities of THC might rely on its keto-enol form and the presence of other THC analogs as impurities. The present study could be advantageous for further research on THC for better understanding its physicochemical properties and biological variation.