Authors:Dustin M. Clifford, Ahmed A. El-Gendy, Amos J. Lu, Dmitry Pestov, and Everett E. Carpenter
Cobalt nanoparticles were synthesized using continuous-flow (CF) chemistry in a stainless steel microreactor for the first time at high output based on the ethanol hydrazine alkaline system (EHAS) producing a yield as high as 1 g per hour [1, 2]. Continuous-flow (CF) synthetic chemistry provides uninterrupted product formation allowing for advantages including decreased preparation time, improved product quality, and greater efficiency. This successful synthetic framework in continuous-flow of magnetic Co nanoparticles indicates feasibility for scaled-up production. The average particle size by transmission electron microscopy (TEM) of the as-synthesized cobalt was 30±10 nm, average crystallite size by Scherrer analysis (fcc phase) was 15±2 nm, and the estimated magnetic core size was 6±1 nm. Elemental surface analysis (X-ray photoelectron spectroscopy [XPS]) indicates a thin CoO surface layer. As-synthesized cobalt nanoparticles possessed a saturation magnetization (Ms) of 125±1 emu/g and coercivity (Hc) of 120±5 Oe. The actual Ms is expected to be greater since the as-synthesized cobalt mass was not weight-corrected (nonmagnetic mass: reaction by-products, solvent, etc.). Our novel high-output, continuous-flow production (>1 g/hr) of highly magnetic cobalt nanoparticles opens an avenue toward industrial-scale production of several other single element magnetic nanomaterials.
Authors:Said A. Hassan, Noha Ibrahim, Eman S. Elzanfaly, and Ahmed E. El Gendy
Chloroquine phosphate (CQ) the antimalarial drug and suggested to treat the pandemic disease coronavirus (COVID-19) is often adulterated with some of the non-steroidal anti-inflammatory drugs (NSAIDs) such as paracetamol, aspirin (ASP), or both. The purpose of this study is to detect such counterfeited drugs, using a reversed phase high pressure liquid chromatography (RP-HPLC) method with fluorescence detection. Analysis was divided into three phases. In the first phase, a Plackett-Burman design (PBD) was used to screen five independent factors, namely, buffer pH, buffer concentration (mM), acetonitrile content (%), flow rate (mL/min) and triethylamine (TEA) content in the buffer preparation (%). The selected dependent variables were (resolution, symmetry of peaks and run time). The objective of the second phase was to optimize the method performance using Box-Behnken design (BBD) and desirability function for multiple response optimization to obtain the best chromatographic performance with the shortest run time. Optimal chromatographic separation was achieved on a YMC-pack pro C18 ODS-A column (15 cm × 4.6 mm, 5 µm) at room temperature The optimum mobile phase consisted of acetonitrile and 5 mM sodium dihydrogen phosphate buffer containing 0.5% triethyamine (30:70, v/v) with the pH adjusted to 3.5 using an orthophosphoric acid solution. The flow rate was maintained at 1 mL/min, and the detection was performed with a fluorescence detector fixed at 380 nm (λemission) after excitation at 335 nm (λexcitation). The third phase was method validation according to ICH guidelines, providing to be specific, precise, accurate, and robust. The method is linear over a range of 0.4–8 µg/mL for chloroquine and ASP, while for paracetamol it is linear over 16–48 µg/mL. The developed RP-HPLC method was used for quantitation of the three drugs in chloroquine dosage form samples. The method shows a great tendency in the classification between the genuine chloroquine and the adulterated ones in pharmaceutical preparations and breast milk.