Katalin Bocz

Comparison of spray drying, electroblowing and electrospinning for preparation of Eudragit E and itraconazole solid dispersions

Three solvent based methods: spray drying (SD), electrospinning (ES) and air-assisted electrospinning (electroblowing; EB) were used to prepare solid dispersions of itraconazole and Eudragit E. Samples with the same API/polymer ratios were prepared in order to make the three technologies comparable. The structure and morphology of solid dispersions were identified by scanning electron microscopy and solid phase analytical methods such as, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman chemical mapping. Moreover, the residual organic solvents of the solid products were determined by static headspace-gas chromatography/mass spectroscopy measurements and the wettability of samples was characterized by contact angle measurement. The pharmaceutical performance of the three dispersion type, evaluated by dissolution tests, proved to be very similar. According to XRPD and DSC analyses, made after the production, all the solid dispersions were free of any API crystal clusters but about 10 wt% drug crystallinity was observed after three months of storage in the case of the SD samples in contrast to the samples produced by ES and EB in which the polymer matrix preserved the API in amorphous state.

In vitro dissolution–permeation evaluation of an electrospun cyclodextrin-based formulation of aripiprazole using μFlux™

Since it is a well-known fact that among the newly discovered active pharmaceutical ingredients the number of poorly water soluble candidates is continually increasing, dissolution enhancement of poorly water soluble drugs has become one of the central challenges of pharmaceutical studies. So far the preclinical studies have been mainly focused on formulation methods to enhance the dissolution of active compounds, in many cases disregarding the fact that the formulation matrix not only affects dissolution but also has an effect on the transport through biological membranes, changing permeation of the drug molecules. The aim of this study was to test an electrospun cyclodextrin-based formulation of aripiprazole with the novel μFlux apparatus, which monitors permeation together with dissolution, and by this means better in vitro-in vivo correlation is achieved. It was evinced that a cyclodextrin-based electrospun formulation of aripiprazole has the potential to ensure fast drug delivery through the oral mucosa owing to the ultrafast dissolution of the drug from the formulation and the enhanced flux across membranes as shown by the result of the novel in vitro dissolution and permeation test.

Flame retardancy of sorbitol based bioepoxy via combined solid and gas phase action

Flame-retarded bioepoxy resins were prepared with the application of commercially available sorbitol polyglycidyl ether (SPE). The additive-type flame retardancy of the cycloaliphatic amine-cured SPE was investigated. Three-percent phosphorus (P)-containing samples were prepared with the application of the liquid resorcinol bis(diphenyl phosphate) (RDP), the solid ammonium polyphosphate (APP), and by combining them. Synergistic effect was found between the inorganic APP and the organophosphorus RDP, when applied in combination: formulations applying RDP or APP alone showed increased limiting oxygen index (LOI) values, however, their UL-94 standard ratings remained HB. When the same amount of P originated from the two additives, V-0, self-extinguishing rating and LOI value of 34% (v/v) was reached. By the combined approach the heat release rate of SPE could be lowered by approximately 60%. The assumed balanced solid and gas phase mechanism was confirmed by thermogravimetric analysis, Fourier transform infrared spectrometry (FTIR) analysis (of the gases formed during laser pyrolysis), attenuated total reflection-infrared spectrometry (ATR-IR) analysis (of the charred residues), as well as by mechanical testing (of the char obtained after combustion).

Key Role of Reinforcing Structures in the Flame Retardant Performance of Self-Reinforced Polypropylene Composites

The flame retardant synergism between highly stretched polymer fibres and intumescent flame retardant systems was investigated in self-reinforced polypropylene composites. It was found that the structure of reinforcement, such as degree of molecular orientation, fibre alignment and weave type, has a particular effect on the fire performance of the intumescent system. As little as 7.2 wt % additive content, one third of the amount needed in non-reinforced polypropylene matrix, was sufficient to reach a UL-94 V-0 rating. The best result was found in self-reinforced polypropylene composites reinforced with unidirectional fibres. In addition to the fire retardant performance, the mechanical properties were also evaluated. The maximum was found at optimal consolidation temperature, while the flame retardant additive in the matrix did not influence the mechanical performance up to the investigated 13 wt % concentration.

Effect of particle size of additives on the flammability and mechanical properties of intumescent flame retarded polypropylene compounds

The effect of particle size reduction of the components of a common intumescent flame retardant system, consisting of pentaerythritol (PER) and ammonium polyphosphate (APP) in a weight ratio of 1 to 2, was investigated on the flammability and mechanical performance of flame retarded polypropylene (PP) compounds. Additives of reduced particle size were obtained by ball milling. In the case of PER, the significant reduction of particle size resulted in inferior flame retardant and mechanical performance, while the systems containing milled APP noticeably outperformed the reference intumescent system containing as-received additives. The beneficial effect of the particle size reduction of APP is explained by the better distribution of the particles in the polymer matrix and by the modified degradation mechanism which results in the formation of an effectively protecting carbonaceous foam accompanied with improved mechanical resistance. Nevertheless, 10% higher tensile strength was measured for the flame retarded PP compound when as-received APP was substituted by milled APP.

Reactive and Additive Phosphorus-based Flame Retardants of Reduced Environmental Impact

Abstract Phosphorus-based flame retardants are environmentally favored owing to their lower environmental impact during their entire life-cycle—including production, use, and disposal—when compared to other conventional flame retardants. Phosphorus-containing flame retardant systems are reviewed in this chapter by presenting the most recent innovative approaches of environmentally friendly flame retardancy. Environment- and process-centered comparison of reactive and additive fire retardant types is presented on the example of thermoplastic polyurethanes. In the case of epoxy resins preferences are given to the novel reactive-type flame retardants, especially when these are synthesized according to the principles of green chemistry. In thermoplastics, where the additive-type flame retardants dominate, the environmental gain of interface/interphase modifications is highlighted. In order to achieve even more green flame retardant systems the use of recycled and renewable resources is proposed.

Fire-retardant recyclable and biobased polymer composites

Abstract This chapter reviews flame retardancy of recyclable and biobased polymer composites. Synthesis routes to obtain thermosetting biobased polymer matrices are discussed and environmentally friendly flame-retardancy solutions are proposed. Fire retardancy of thermoplastic biomatrices and fully recyclable self-reinforced composites made thereof are summarized. New methods to characterize flame-retardant biocomposites and understand their thermal degradation and flame-retardant mechanisms are presented. After reviewing chemical treatments to flame retard natural fibres, flame-retardancy results of thermosetting and thermoplastic biocomposites are discussed. Green solutions utilizing synergistic effects, multifunctionality and integrated approaches are highlighted. Finally, application possibilities and future trends in the field of flame-retarded biocomposites are indicated.

Application of Melt-Blown Poly(lactic acid) Fibres in Self-Reinforced Composites

The aim of our research was to produce poly(lactic acid) (PLA) fibres with diameters in the micrometer size range, serving as the reinforcing phase in self-reinforced (SR) PLA composites. Nonwoven PLA mats were manufactured by solvent-free melt-blowing technology. Three types of PLA differing in d-lactide content were processed with a productivity as high as 36 g/h. The crystallinity of the PLA microfibres was enhanced by thermal annealing. A 2–3-fold increase in the degree of crystallinity was obtained, as measured by differential scanning calorimetry (DSC). Fibre diameters between 2–14 µm were revealed by scanning electron microscopy (SEM). Static tensile tests were performed on the nonwoven mats, showing the reduced moduli of the annealed fibres due the amorphous relaxation. The PLA mats were processed via the hot compaction technique and formed into SR–PLA composites. The morphological and mechanical properties of the obtained microstructural composites were comprehensively studied. Composites prepared from annealed, thermally more stable PLA nonwoven mats showed superior mechanical properties; the tensile strength improved by 47% due to the higher residual fibre content.