Browsing by Author "Hegazy M.A."

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Comparative study of reversed-phase high-performance liquid chromatography versus thin-layer chromatography-densitometry for determination of Citicoline sodium in presence of its alkaline degradation products
(Akademiai Kiado Rt., 2015) Mahmoud O.A.; Hegazy M.A.; Salem H.; Moustafa A.A.; Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); October City; 11787; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt
Simple, sensitive, selective, and precise stability-indicating thin-layer chromatography (TLC)-densitometric and reversed-phase high-performance liquid chromatography (RP-HPLC) methods were developed and validated for the determination of citicoline sodium (CT) in the presence of its alkaline degradation products (CT Deg.) and in pharmaceutical oral solution. TLC-densitometry employs aluminum TLC plates precoated with silica gel 60 F254 as the stationary phase and ammonia-ethyl acetate-triethylamine (6:3.5:0.5, v/v) as the mobile phase to give compact spots for citicoline sodium (RF = 0.35) and its degradation product (RF = 0.1); the chromatogram was scanned at 272 nm. RP-HPLC utilizes a C18 column and a mobile phase consisting of methanol-water-acetic acid (60:40:0.1, v/v); the pH level was adjusted to 4 using 0.1% orthophosphoric acid, at a flow rate of 1 mL min-1 for the separation of citicoline sodium (tR = 1.801) and its degradation product (tR = 3.422). Quantitation was achieved by ultraviolet (UV) detection at 272 nm. Citicoline sodium was exposed to alkaline hydrolysis, and a comparative study was carried out to show the advantages of the proposed chromatographic methods in determination of citicoline sodium in the presence of its alkaline degradation products. The chromatographic methods were developed and validated as per the International Conference on Harmonization guidelines. As the methods could effectively separate the drug from their degradation products, these techniques can be employed as stability-indicating methods that have been successively applied to pharmaceutical formulations without interference from the excipients. � Akad�miai Kiad�, Budapest.
Evaluation of multivariate calibration models with different pre-processing and processing algorithms for a novel resolution and quantitation of spectrally overlapped quaternary mixture in syrup
(Elsevier, 2016) Moustafa A.A.; Hegazy M.A.; Mohamed D.; Ali O.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); 6th October City11787; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt
A novel approach for the resolution and quantitation of severely overlapped quaternary mixture of carbinoxamine maleate (CAR), pholcodine (PHL), ephedrine hydrochloride (EPH) and sunset yellow (SUN) in syrup was demonstrated utilizing different spectrophotometric assisted multivariate calibration methods. The applied methods have used different processing and pre-processing algorithms. The proposed methods were partial least squares (PLS), concentration residuals augmented classical least squares (CRACLS), and a novel method; continuous wavelet transforms coupled with partial least squares (CWT-PLS). These methods were applied to a training set in the concentration ranges of 40-100 ?g/mL, 40-160 ?g/mL, 100-500 ?g/mL and 8-24 ?g/mL for the four components, respectively. The utilized methods have not required any preliminary separation step or chemical pretreatment. The validity of the methods was evaluated by an external validation set. The selectivity of the developed methods was demonstrated by analyzing the drugs in their combined pharmaceutical formulation without any interference from additives. The obtained results were statistically compared with the official and reported methods where no significant difference was observed regarding both accuracy and precision. 2015 Elsevier B.V. All rights reserved.
Functionalized Fe3O4 Magnetic Nanoparticle Potentiometric Detection Strategy versus Classical Potentiometric Strategy for Determination of Chlorpheniramine Maleate and Pseudoephedrine HCl
(Hindawi Limited, 2019) Moustafa A.A.; Hegazy M.A.; Mohamed D.; Ali O.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); 6th October City; 11787; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt
Nanosized adsorbents when used in potentiometric methods of analysis usually show better performance rather than the traditional potentiometric approach; this is attributed to the high specific surface area of the nanomaterial used in addition to the lack of internal diffusion resistance, thus improving their adsorption capacity. In the presented work, a rapid and sensitive potentiometric determination of chlorpheniramine maleate (CPM) and pseudoephedrine hydrochloride (PSE) in pure form, in pharmaceutical preparation, and in biological fluid was developed based on functionalized magnetic nanoparticles (Fe3O4). This strategy was compared with the classical potentiometric strategy. Three types of sensors were constructed using phosphotungstic acid (PTA), ?-cyclodextrin (?-CD), and ?-cyclodextrin-conjugated Fe3O4 magnetic nanoparticles for the potentiometric determination of each of CPM and PSE. The prepared sensors were characterized in regards to their composition, life duration, working pH range, and response time. The sensors have demonstrated promising selectivity to CPM and PSE in the presence of pharmaceutical formulation excipients, plasma matrix, and a diversity of both organic and inorganic interfering materials. The developed sensors have displayed good responses. Statistical comparison of the achieved results with a reported method has revealed no significant difference regarding both accuracy and precision. � 2019 Azza A. Moustafa et al.
Liquid chromatography–tandem MS/MS method for simultaneous quantification of paracetamol, chlorzoxazone and aceclofenac in human plasma: An application to a clinical pharmacokinetic study
(John Wiley and Sons Ltd, 2018) Mohamed D.; Hegazy M.A.; Elshahed M.S.; Toubar S.S.; Helmy M.I.; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Cairo; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; 6 October City; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Cairo; Egypt
A facile, fast and specific method based on liquid chromatography�tandem mass spectrometry (LC�MS/MS) for the simultaneous quantitation of paracetamol, chlorzoxazone and aceclofenac in human plasma was developed and validated. Sample preparation was achieved by liquid�liquid extraction. The analysis was performed on a reversed-phase C18 HPLC column (5 ?m, 4.6 � 50 mm) using acetonitrile�10 mM ammonium formate pH 3.0 (65:35, v/v) as the mobile phase where atrovastatin was used as an internal standard. A very small injection volume (3 ?L) was applied and the run time was 2.0 min. The detection was carried out by electrospray positive and negative ionization mass spectrometry in the multiple-reaction monitoring mode. The developed method was capable of determining the analytes over the concentration ranges of 0.03�30.0, 0.015�15.00 and 0.15�15.00 ?g/mL for paracetamol, chlorzoxazone and aceclofenac, respectively. Intraday and interday precisions (as coefficient of variation) were found to be ?12.3% with an accuracy (as relative error) of �5.0%. The method was successfully applied to a pharmacokinetic study of the three analytes after being orally administered to six healthy volunteers. Copyright � 2018 John Wiley & Sons, Ltd.
Novel Approach for the Simultaneous Determination of Carbinoxamine Maleate, Pholcodine, and Ephedrine Hydrochloride Without Interference from Coloring Matter in an Antitussive Preparation Using Smart Spectrophotometric Methods
(2018) Moustafa A.A.; Hegazy M.A.; Mohamed D.; Ali O.; Cairo University; Faculty of Pharmacy; Analytical Chemistry Department; Kasr-El Aini St; 11562 Cairo; Egypt; October University for Modern Sciences and Arts; Faculty of Pharmacy; Analytical Chemistry Department; 11787 6th of October City; Egypt Helwan University; Faculty of Pharmacy; Analytical Chemistry Department; Ein Helwan; 11795 Cairo; Egypt; October University for Modern Sciences and Arts; Faculty of Pharmacy; Analytical Chemistry Department; 11787 6th of October City; Egypt
The presence of coloring matters in syrups usually interferes with the spectrophotometric determination of active pharmaceutical ingredients. A novel approach was introduced to eliminate the interference of sunset yellow (coloring matter) in Cyrinol syrup. Smart, simple, accurate, and selective spectrophotometric methods were developed and validated for the simultaneous determination of a ternary mixture of carbinoxamine maleate, pholcodine, and ephedrine hydrochloride in syrup. Four of the applied methods used ratio spectra: successive derivative subtraction coupled with constant multiplication, successive derivative of ratio spectra, ratio subtraction coupled with ratio difference, and ratio spectra continuous wavelet transforms zero-crossing. In addition, a method that was based on the presence of an isosbestic point, the amplitude summation method, was also established. A major advantage of the proposed methods is the simultaneous determination of the mentioned drugs without prior separation steps. These methods were successfully applied for the determination of laboratory-prepared mixtures and a commercial pharmaceutical preparation without interference from additives, thus proving the selectivity of the methods. No significant difference regarding both accuracy and precision was observed upon statistical comparison of the results obtained by the proposed methods with each other and with those of official or reported ones.
Novel contribution to the simultaneous monitoring of pramipexole dihydrochloride monohydrate and levodopa as co-administered drugs in human plasma utilizing UPLC-MS/MS
(SAGE Publications Ltd, 2018) Mohamed D.; Hegazy M.A.; Elshahed M.S.; Toubar S.S.; Helmy M.I.; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Cairo; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; 6 October City; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Cairo; Egypt
An efficient, selective, sensitive, and rapid ultra-performance liquid chromatography tandem mass spectrometry method was established and validated for the quantification of pramipexole dihydrochloride monohydrate and levodopa simultaneously in human plasma with the aid of diphenhydramine as an internal standard. A simple protein precipitation technique with HPLC grade acetonitrile was efficiently utilized for the cleanup of plasma. The analysis was performed using a Hypersil gold 50 mm � 2.1 mm (1.9 �m) column and a mobile phase of 0.2% formic acid and methanol (90: 10 v/v). The triple-quadrupole mass spectrometer equipped with an electrospray source operated in the positive mode was set up in the selective reaction monitoring mode (SRM) to detect the ion transitions m/z 212.15 ?153.01, m/z 198.10? 135.16, and m/z 255.75 ? 166.16 for pramipexole dihydrochloride monohydrate, levodopa, and diphenhydramine, respectively. The method was thoroughly validated according to FDA guidelines and proved to be linear, accurate, and precise over the range 100-4000 pg/mL for pramipexole dihydrochloride monohydrate and 60-4000 ng/mL for levodopa. The proposed method was effectively applied for monitoring both drugs in plasma samples of healthy volunteers. The Author(s) 2018.
Simultaneous quantification of chlorpheniramine, pseudoephedrine, and ibuprofen in antitussive preparation by high-performance liquid chromatography and thin-layer chromatography densitometric methods
(Akademiai Kiado Rt., 2018) Moustafa A.A.; Hegazy M.A.; Mohamed D.; Ali O.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA)11787; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt
Simple, accurate, precise, sensitive, and validated high-performance liquid chromatography (HPLC) and thin-layer chromatography (TLC)?densitometric methods were developed for the simultaneous determination of chlorpheniramine maleate (CPM), pseudoephedrine HCl (PSE), and ibuprofen (IBF) in tablet dosage form. In method A, reversed-phase (RP)-HPLC analysis was performed on Zorbax C8 column (150 mm 4.6 mm, 5 m particle size i.d.), using a mobile phase consisting of methanol acetonitrile distilled water (pH 4) using orthophosphoric acid in the ratio (80:10:10, v/v) and flow rate of 0.7 mL min-1. Quantification was achieved with ultraviolet (UV) detection at 220 nm. In method B, TLC analysis was carried out on an aluminum-backed sheet of silica gel 60 F254 layer using ethyl acetate?methanol?ammonia (8:2:0.8, v/v) as the mobile phase. Quantification was carried out with UV detection at 262 nm. The validation of the proposed methods was applied according to the International Conference on Harmonization (ICH) guidelines. The suggested methods were successfully applied for the determination of the cited drugs in bulk powder and commercial dosage form. Akadmiai Kiad, Budapest.
Simultaneous spectrophotometric determination of overlapping spectra of paracetamol and caffeine in laboratory prepared mixtures and pharmaceutical preparations using continuous wavelet and derivative transform
(Analytical & Bioanalytical Electrochemistry, 2015) Ashour A.; Hegazy M.A.; Abdel-Kawy M.; ElZeiny M.B.; Department of Analytical Chemistry; Faculty of Pharmacy; Misr International University; Egypt; Department of Analytical Chemistry; Faculty of Pharmacy; Cairo University; Egypt; Department of Analytical Chemistry; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); Egypt
In the present paper, two spectrophotometric methods were used for the simultaneous analysis of paracetamol (PCT) and caffeine (CAF) in their laboratory prepared mixtures and pharmaceutical preparations. Simple spectrophotometric analysis of PCT and CAF is not possible due to their complete spectral overlap. The proposed methods are based on the application of continuous wavelet transform (CWT) and derivative transform (using Savitsky-Golay filters) on the ratio spectra to predict each of CAF and PCT. Several wavelet families were tested. Coif1 and Sym2 were found to give best results under optimum conditions. The transformed signals of ratio spectra were used to plot the calibration curves for both components. The predictability of the built calibrations was validated through their application on several synthetic mixtures of both drugs. The proposed methods were used for the prediction of CAF and PCT in pharmaceutical preparation. The obtained results were statistically compared to a reference HPLC method. No significant differences were found between the obtained results and those from the reference method. Being simple, rapid, cheap and sensitive, the proposed methods are recommended for the routine daily analysis of these two drugs in their mixtures in quality control laboratories. � 2012.