Compatibility study between indomethacin and excipients in their physical mixtures

Thermal analysis is a routine method for analysis of drugs and substances of pharmaceutical interest. Thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) are thermoanalytical methods which offer important information about the physical and chemical properties of drugs (purity, stability, phase transition, polymorphism, compatibility, kinetic analysis, etc.). This work exemplifies a general method of studying the drug-excipient interactions with the aim of predicting rapidly and inexpensively the long thermal stability of their mixtures. The TG/DTG and DSC were used as screening techniques for assessing the compatibility between indomethacin (IND) and its physical associations as binary mixtures with some common excipients. Based on their frequent use in preformulations eleven different excipients: corn starch, microcrystalline cellulose (PH 101; PH 102), colloidal silicon dioxide, lactose (monohydrate and anhydre), polyvinilpyrrolidone K30, magnesium stearate, talc, stearic acid, and manitol were blended with IND. The samples were prepared by mixing the analyte and excipients in a proportion of 1:1 (w:w). In order to investigate the possible interactions between the components, the thermal curves of IND and each selected excipient were compared with those of their 1:1 (w/w) physical mixtures. FT-IR spectroscopy and X-ray powder diffraction were used as complementary techniques to adequately implement and assist in interpretation of thermal results. On the basis of thermal results, confirmed by FT-IR and X-ray analyses, a possible interaction was found between IND with polyvinylpyrrolidone K30, magnesium stearate, and stearic acid.     

Thermal analysis of new glycopolymers derived from monosaccharides

A novel monomer carrying carbohydrate moiety was prepared by simple reaction of methacrylic acid with 3-O-(2′,3′-epoxy-propyl)-1,2:5,6-di-O-isopropylidene-α-d-glucofuranose. Another d-glucose oligomer was synthesized by the polycondensation of a dicarboxylic acid including the carbohydrate residue into the main polymeric chain, 3-O-benzyl-5,6-(bis-O-(acryloyloxy))-1,2-di-O-isopropylidene-α-d-glucofuranose, with propane-1,3-diol using p-toluenesulfonic acid as catalyst. These products were copolymerized with styrene and 2-hydroxypropyl methacrylate, respectively, at different mass ratios, using benzoyl peroxide as initiator. Differential scanning calorimetry was performed in order to study the copolymerization process of the monomer and oligomer into the chosen co-monomers, respectively, and the activation energy of this process was evaluated using Kissinger–Akahira–Sunose (KAS) method. The storage and loss modulus of the obtained glycopolymers were evaluated using dynamic mechanical analysis. The thermal stability of the obtained products was studied via thermogravimetry.     

Compatibility study between ibuprofen and excipients in their physical mixtures

The thermal techniques of analysis were used to assess the compatibility between ibuprofen (IB) and some excipients used in the development of extended released formulations. This study is a part of a systematic study undertaken to find and optimizes a general method of detecting the drug–excipient interactions, with the aim of predicting rapidly and assuring the long-term stability of pharmaceutical product and speeding up its marketing. The thermal properties of IB and its physical association as binary mixtures with some common excipients were evaluated by thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry. FT-IR spectroscopy and X-ray powder diffraction (XRPD) were used as complementary techniques to adequately implement and assist in interpretation of the thermal results. Based on their frequent use in preformulations nine different excipients: starch; microcrystalline cellulose (PH 101 and PH 102); colloidal silicon dioxide; lactose (monohydrate and anhydre); polyvinylpyrrolidone; magnesium stearate and talc were blended with IB. The samples were prepared by mixing the analyte and excipients in a proportion of 1:1 (w:w). The TG/DSC curves of the IB have shown a single stage of mass loss between 175 and 290 °C, respectively, an endothermic peak at 78.5 °C, which corresponds to the melting (literature T _m = 75–78 °C).     

Capillary-HPLC-ESI-MS/MS method for the determination of acidic products from the oxidation of monoterpenes in atmospheric aerosol samples

A method is presented for the determination of acidic products from terpene oxidation in filter samples of the atmospheric particle phase. Oxidation products of monoterpenes are believed to add a large fraction to the secondary organic aerosol (SOA) in the troposphere. Those products with structures containing one or more carboxylic acid groups have especially low vapour pressures and therefore they are believed to contribute substantially to the particle phase. Although many experiments were performed in simulation chambers to study the SOA generation by oxidation of terpenes, concentration measurements of products in the atmospheric particle phase are still rare. This is especially true for oxidation products of terpenes other than α- and β-pinene. Therefore, we developed a method for the quantification of acidic products from terpene oxidation in atmospheric aerosol samples. After passing a PM 2.5 (PM = particulate matter) pre-separator to remove coarse particles, fine atmospheric particles were collected onto quartz fibre filters. A backup filter was placed behind the first filter to estimate possible sampling artifacts. The filters were extracted in an ultrasonic bath using methanol. After enrichment and re-dissolving in water the samples were analysed using a capillary-HPLC-ESI(−)-MSⁿ set-up. The ion trap mass spectrometer could be used to gain structural information about the analytes and to enhance the selectivity of the measurements by using its MS/MS capability. A variety of products from different terpenes could be identified and quantified in samples of the ambient atmosphere using reference data from chamber experiments. Due to strong matrix effects quantification of samples from the real atmosphere had to be done by the standard addition method.     

Characterization of iodine species in the marine aerosol: To understand their roles in particle formation processes

In this contribution, iodine chemistry in the Marine Boundary Layer (MBL) is introduced. A series of methodologies for the measurements of iodine species in the gas and particle phases of the coastal atmosphere has been developed. Iodine species in the gas phase in real air samples has been determined in two field campaigns at the west coast of Ireland, indicating that gaseous iodo-hydrocarbons and elemental iodine are the precursors of new particle formation. Particulate iodine speciation from the same measurement campaigns show that the non-water-soluble iodine compounds are the main iodine species during the marine particle formation. A seaweed-chamber experiment was performed, indicating that gaseous I₂ is one of the important precursors that lead to new particle formation in the presence of solar light in the ambient air at the coastal tidal area.     

Thermal behavior of oligo[(ε-caprolactone)-co-δ-gluconolactone] enzymatically synthesized in reaction conditions optimized by experimental design

Journal of Thermal Analysis and Calorimetry - The thermal behavior of co-oligomers of ε-caprolactone (ECL) with gluconolactone, compared to the ε-caprolactone oligomer, has been assessed...     

Thermal stability and biodegradation of novel D-mannose based glycopolymers

This paper presents the thermal stability and biodegradability testing of new glycopolymers obtained by copolymerization of a novel D-mannose based oligomer with 2-hydroxypropyl acrylate and 2-hydroxypropyl methacrylate. The thermal analysis of these glycopolymers was investigated by thermogravimetry and the glass transition temperature was determined by DSC. While the acrylate derived glycopolymer has values of the glass transition temperature below 0 °C, the methacrylate derivative has positive values, above 50 °C. The biodegradation studies of the glycopolymers were carried out in a liquid medium, using pure cultures of two microorganisms, Zymomonasmobilis and Trichodermareesei. The weight losses of the new plastic materials were significant (almost 40%) and the best results were assessed for the 2-hydroxypropyl acrylate glycopolymer in the presence of both Z. mobilis and T. reesei. Microscopy showed that both microorganisms were present on the surface of the new glycopolymers and developed small colonies while modifying their surface. The changes inside the morphology of the polymeric materials structure were drastic and were studied via SEM analysis.     

Electronic absorption spectra,ESR spectra,and structure of coordination polyhedrons of titanium(III) in molten and “instantly cooled” systems of sodium phosphates and halides

The structure of Ti(III) coordination polyhedrons in both individual NaPO₃ and 70 mole % NaPO₃-30 mole % Na_nX mixtures (X=PO₃ ^3–, P₂O₇ ^4–, F^–, Cl^–) in the molten and solid states has been investigated on the basis of data from electronic absorption and ESR spectra. The formation of tetragonally distorted Ti(III) coordination polyhedrons with D_4h symmetry coordinated only by (PO₃ ^–)_n chains with the following values of the spectroscopic parameters for the molten (and solid) states has been established in all the phosphate systems investigated: 10Dq=17,300 (18,000) cm^–1 (Ds=50 cm^–1, Dt=5600, g=1.959, g₁=1.930, =93. cm^–1). It has been shown that the greater is the extent of depolymerization of the phosphate chains in the melt, the stronger is the Ti(III) coordination polyhedron formed; the following relative series of the depolymerizing strength of the anions has accordingly been established: PO₄ ^3–2O₇ ^4–––.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 5, pp. 610–614, September–October, 1989.     

Mass spectrometric investigation of reactions of oxygen exchange and partial oxidation of methane in molten catalysts

This work has been devoted to a mass spectrometric investigation of the interaction of atmospheric oxygen or an air-methane mixture with molten V₂O₅-NaPO₃, selected as a model catalyst; the work has been further aimed at studying the reaction mechanisms. The data on the change in isotope composition¹⁸O/¹⁶O have been analyzed, and the rate constants and order of reaction with respect to oxygen have been determined.A mechanism has been proposed for the interaction of both atmospheric oxygen and the air-methane mixture with the melt.Institute of General and Inorganic Chemistry, Academy of Sciences of the Ukrainian SSR, Kiev. Translated from Teoreticheskaya i Éksperimental'naya Khimiya, No. 1, pp. 99–104, January–February, 1991. Original article submitted May 3, 1990.