Browsing by Author "Khattab F.I."
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Item Determination of fluoroquinolone antibiotics in industrial wastewater by high-pressure liquid chromatography and thin-layer chromatography-densitometric methods(Akademiai Kiado Rt., 2014) Khattab F.I.; Salem H.; Riad S.M.; Elbalkiny H.T.; Cairo University; Analytical Chemistry Department; Faculty of Pharmacy; Kasr-El Aini Street; 11562 Cairo; Egypt; October University for Modern Sciences and Arts (MSA); Analytical Chemistry Department; Faculty of Pharmacy; 11787 6th October City; EgyptTwo methods were described for the simultaneous determination of ciprofloxacin HCl (CIP) and moxifloxacin HCl (MOX) in their binary mixture present in industrial wastewater. A solid-phase extraction procedure (SPE) based on retention on HLB OASIS cartridges and elution with a mixture of methanol-water in acidic medium was preformed, and then both fluoroquinolones were separated using two chromatographic methods. The first method was based on high-performance liquid chromatographic separation of the two drugs on reversed-phase Zorbax C18 column. The mobile phase consisted of monobasic potassium phosphate (50 mM, pH 2.5, adjusted with phosphoric acid) and acetonitrile (80:20, v/v). Flow rate was 1 mL min-1. Quantitation was achieved with ultraviolet (UV) detection at 278 nm. Linearity was found to be over the concentration range of 1-50 ?g mL-1 for both CIP and MOX. The second method was based on the thin-layer chromatographic (TLC) separation of the two drugs followed by densitometric measurements of their bands at 278 nm. The separation was carried out on silica gel 60 F254 plates, using methanol, ammonia, and methylene chloride (55:35:20, v/v) as a developing system. The linearity was found to be in the range of 0.25-2.5 ?g band -1 for both CIP and MOX. Both methods were optimized and validated as per International Conference on Harmonization (ICH) guidelines. Separation was developed on spiked water samples and checked on process wastewaters of industrial origin after SPE sample pretreatment.Item Ion-Selective membrane sensors for the determination of ciprofloxacin hydrochloride in water and pharmaceutical formulation(Center of Excellence in Electrochemistry, Univ. of Tehran, 2014) Riad S.M.; Khattab F.I.; Salem H.; Elbalkiny H.T.; Analytical Chemistry Department; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Analytical Chemistry Department; October University for Modern Sciences and Arts (MSA); 6th October City; 11787; EgyptThe construction and electrochemical response characteristics of six Ciprofloxacin-selective electrodes were investigated using precipitation based technique with sodium tetraphenyl borate (TPB), phosphomolybdate (PMA) and phosphotungstate (PTA); respectively upon using polyvinyl chloride (PVC) matrix and dibutyl phthalate (DBP) as a plasticizer. The resultant sensors have different forms, either as membrane electrodes (sensors 1, 3 and 5) or as coated wire electrodes (sensors 2, 4 and 6). Linear responses of CIP within the concentration ranges of 10?6 to 10?2 mol/L for sensors 1, 2 and 5 while for sensors 3 and 4, the linear responses were within the concentration ranges of 10?5 to 10?2 mol/L and for sensor 6 it shows linear responses within the concentration ranges of 10?7 to 10?2 mol/L. Nernstian slopes of 51.7, 50.7, 58.3, 57.7, 44 and 41.8 mV/decade were observed over the pH range of (5�9) for sensors 1, 2, 5 and 6 and over range of (5-7) for sensor 3 and 4 respectively. The selectivity coefficients of the developed sensors indicated excellent selectivity for CIP. The proposed sensors displayed useful analytical characteristics for the determination of CIP in water samples and pharmaceutical preparation. 2014 by CEE.Item Validated univariate and multivariate spectrophotometric methods for the determination of pharmaceuticals mixture in complex wastewater(Blackwell Publishing Ltd, 2015) Riad S.M.; Salem H.; Elbalkiny H.T.; Khattab F.I.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Deraya University; Menia; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); October City; 11787 6th; EgyptFive, accurate, precise, and sensitive univariate and multivariate spectrophotometric methods were developed for the simultaneous determination of a ternary mixture containing Trimethoprim (TMP), Sulphamethoxazole (SMZ) and Oxytetracycline (OTC) in waste water samples collected from different cites either production wastewater or livestock wastewater after their solid phase extraction using OASIS HLB cartridges. In univariate methods OTC was determined at its ?max 355.7 nm (0D), while (TMP) and (SMZ) were determined by three different univariate methods. Method (A) is based on successive spectrophotometric resolution technique (SSRT). The technique starts with the ratio subtraction method followed by ratio difference method for determination of TMP and SMZ. Method (B) is successive derivative ratio technique (SDR). Method (C) is mean centering of the ratio spectra (MCR). The developed multivariate methods are principle component regression (PCR) and partial least squares (PLS). The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures containing different ratios of the three drugs. The obtained results are statistically compared with those obtained by the official methods, showing no significant difference with respect to accuracy and precision at p = 0.05. � 2015 Elsevier B.V. All rights reserved.