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Design of experiments in optimization and validation of hydrophilic interaction liquid chromatography method for determination of amlodipine besylate and its impurities

100%

Kasagić-Vujanović I. , Knežević D.

Acta Chromatographica

2022

tom Vol. 34, no. 1

41--52

A new and rapid hydrophilic interaction liquid chromatographic method has been developed for the quantitative analysis of amlodipine besylate and its specific impurities (D, E, and F). For development of this method, a systematic approach which includes Design of Experiments methodology was applied. For the method optimization, Box–Behnken design and specific way Derringer’s desirability function were applied. They provided identification of the optimal chromatographic conditions on the basis of obtained mathematical models and graphical procedures (three D graphs). The optimal chromatographic conditions were the analytical column ZORBAX NH2 (250 3 4.6 mm, 5 mm particle size); mobile phase consisted of acetonitrile-water phase (50 mM ammonium acetate, pH adjusted to 4.0 with glacial acetic acid) (90.5:9.5 v/v); column temperature 30 8C, mobile phase flow rate 1 mL min1, wavelength of detection 230 nm. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of amlodipine besylate and its impurities in any laboratory under different circumstances has been proven.

Thermobaric Effects of Cast Composite Explosives of Different Charge Masses and Dimensions

61%

Simić D. , Andjelić U. , Knežević D. , Savić K. , Draganić V. , Sirovatka R. , Tomić L.

Central European Journal of Energetic Materials

2016

tom Vol. 13, no. 1

161--182

The aim of this research was to determine the thermobaric effect of cast composite explosives, with different masses and dimensions of the chosen explosive charges. This was done by measuring the shock wave parameters in air (maximum overpressure and pressure impulse) and quantifying the thermal effect (temperature-time dependence), at different distances from the centre of the detonation. The chosen thermobaric explosive composition, TBE-3, was characterized. Its density, detonation velocity and viscosity-time dependence were determined. Experimental samples of different masses and calibres were prepared. The shock wave parameters in air were determined in field tests, by measuring the overpressure by piezo-electric pressure transducers. The detonation and the expansion of the explosion products were filmed by a TV high-speed camera, Phantom V9. An infrared (IR) camera FLIR SC7200 was used for recording the IR scene of the explosions and for tracking the thermal effects by a thermographic technique, i.e. thermal imaging. This work is an initial step towards establishing a method for the quantification of the thermal effects of a thermobaric detonation.