Browsing by Author "Mohamed D."

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A comparative study of smart spectrophotometric methods for simultaneous determination of a skeletal muscle relaxant and an analgesic in combined dosage form
(Elsevier, 2015) Salem H.; Mohamed D.; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; October City; 11787 6; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Deraya University; Cairo; 14511; Egypt
Six simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the analgesic drug; paracetamol (PARA) and the skeletal muscle relaxant; dantrolene sodium (DANT). Three methods are manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and mean centering (MC). The other three methods are utilizing the isoabsorptive point either at zero order namely; absorbance ratio (AR) and absorbance subtraction (AS) or at ratio spectrum namely; amplitude modulation (AM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined dosage form. Standard deviation values are less than 1.5 in the assay of raw materials and capsules. The obtained results were statistically compared with each other and with those of reported spectrophotometric ones. The comparison showed that there is no significant difference between the proposed methods and the reported methods regarding both accuracy and precision. � 2015 Elsevier B.V. All rights reserved.
A comparative study of smart spectrophotometric methods for simultaneous determination of sitagliptin phosphate and metformin hydrochloride in their binary mixture
(Elsevier, 2015) Lotfy H.M.; Mohamed D.; Mowaka S.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmaceutical Sciences and Pharmaceutical Industries; Future University; Cairo; 12311; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; October City; 117876; Egypt; Department of Analytical Chemistry; Faculty of Pharmacy; British University in Egypt; El-Sherouk City; 11837; Egypt
Simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the oral antidiabetic drugs; sitagliptin phosphate (STG) and metformin hydrochloride (MET) in combined pharmaceutical formulations. Three methods were manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and a novel approach of induced amplitude modulation (IAM) methods. The first two methods were used for determination of STG, while MET was directly determined by measuring its absorbance at ?max 232 nm. However, (IAM) was used for the simultaneous determination of both drugs. Moreover, another three methods were developed based on derivative spectroscopy followed by mathematical manipulation steps namely; amplitude factor (P-factor), amplitude subtraction (AS) and modified amplitude subtraction (MAS). In addition, in this work the novel sample enrichment technique named spectrum addition was adopted. The proposed spectrophotometric methods did not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined pharmaceutical formulations. Standard deviation values were less than 1.5 in the assay of raw materials and tablets. The obtained results were statistically compared to that of a reported spectrophotometric method. The statistical comparison showed that there was no significant difference between the proposed methods and the reported one regarding both accuracy and precision. � 2015 Elsevier B.V. All rights reserved.
Different mathematical processing of absorption, ratio and derivative spectra for quantification of mixtures containing minor component: An application to the analysis of the recently co-formulated antidiabetic drugs; canagliflozin and metformin
(Elsevier B.V., 2018) Lotfy H.M.; Mohamed D.; Elshahed M.S.; Pharmaceutical Chemistry Department; Faculty of Pharmaceutical Sciences & Pharmaceutical Industries; Future University in Egypt; Cairo; 12311; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts11787; Egypt
In the presented work several spectrophotometric methods were performed for the quantification of canagliflozin (CGZ) and metformin hydrochloride (MTF) simultaneously in their binary mixture. Two of these methods; response correlation (RC) and advanced balance point-spectrum subtraction (ABP-SS) were developed and introduced for the first time in this work, where the latter method (ABP-SS) was performed on both the zero order and the first derivative spectra of the drugs. Besides, two recently established methods; advanced amplitude modulation (AAM) and advanced absorbance subtraction (AAS) were also accomplished. All the proposed methods were validated in accordance to the ICH guidelines, where all methods were proved to be accurate and precise. Additionally, the linearity range, limit of detection and limit of quantification were determined and the selectivity was examined through the analysis of laboratory prepared mixtures and the combined dosage form of the drugs. The proposed methods were capable of determining the two drugs in the ratio present in the pharmaceutical formulation CGZ:MTF (1:17) without the requirement of any preliminary separation, further dilution or standard spiking. The results obtained by the proposed methods were in compliance with the reported chromatographic method when compared statistically, proving the absence of any significant difference in accuracy and precision between the proposed and reported methods. � 2017 Elsevier B.V.
Enhanced HPLC-MS/MS method for the quantitative determination of the co-administered drugs ceftriaxone sodium and lidocaine hydrochloride in human plasma following an intramuscular injection and application to a pharmacokinetic study
(John Wiley and Sons Ltd, 2018) Mohamed D.; Kamal M.; 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; Al-Ahram Canadian University; 6 October City; Egypt
A sensitive HPLC�MS/MS method was established for the quantification of ceftriaxone sodium (CFT) and lidocaine HCl (LDC) in human plasma utilizing cefixime (CFX) and tadalafil (TDA) as internal standards. The analytes were extracted from human plasma by protein precipitation using acetonitrile. Chromatographic separation was performed on Kinetex C18 (50.0 � 4.6 mm, 5 ?m particle size) column with methanol�0.01�M ammonium acetate pH 6.4 (70: 30, v/v) as mobile phase. Multiple reaction monitoring involving the transitions 555.10 ? 396.20, 235.20 ? 86.00, 454.20 ? 284.80 and 390.20 ? 268.20 was utilized to quantify CFT, LDC, CFX and TDA, respectively, using a triple quadrupole mass spectrometer which was operated in positive ion mode. The method revealed linearity in the concentration range of 3.0�300.0 ?g/mL for CFT and 3.0�300.0 ng/mL for LDC. The validation of the method was achieved in accordance to the US Food and Drug Administration guidelines. A pharmacokinetic study was performed on healthy Egyptian volunteers after intramuscular injection of sterile ceftriaxone sodium (1 g CFT dissolved in 3.5 mL of 1% LDC) after approval from the ethics committee. The pharmacokinetic parameters were: Cmax 141.15 � 39.84 (?g/mL) and 55.02 � 9.36 (ng/mL); tmax (h) 2.50 � 0.50 and 1.5 � 0.50; t� (h) 7.30 � 2.98 and 4.23 � 1.96; and Kel (h?1) 0.10 � 0.04 and 0.20 � 0.13 for CFT and LDC, respectively. � 2018 John Wiley & Sons, Ltd.
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.
Lanthanide-DNA probe for spectrofluorimetric determination of some 6-fluoroquinolones in eye-ear pharmaceutical preparations
(Elsevier Inc., 2019) Rizk M.; Habib I.H.I.; Mohamed D.; Mowaka S.; El-Eryan R.T.; Department of Analytical Chemistry; Faculty of Pharmacy; Helwan University; Ein-Helwan; 11745; Egypt; Department of Applied Organic Chemistry; Microanalytical Chemistry Laboratory; National Research Centre; Dokki; Giza; 12622; Egypt; Department of Pharmaceutical Analytical Chemistry; Faculty of Pharmacy; October University for Modern Sciences and Arts; October City 6; 11787; Egypt; Department of Analytical Chemistry; Faculty of Pharmacy; British University in Egypt; El-Sherouk City; 11837; Egypt
A sensitive, accurate and precise spectrofluorimetric method was established for the quantification of ciprofloxacin HCl and norfloxacin drugs. The spectrofluorimetric method has involved the development of a ternary complex between the investigated drugs and Tb3+ in presence of Calf thymus DNA which was used as a fluorescence enhancing agent causing reduction in the non-radiative energy loss produced by O[sbnd]H vibration of H2O in the original Tb3+�drug complex. Thus, the fluorescence of the system (Tb3+�drug�DNA) at ?em of 545 nm for ?ex of 272 nm was enhanced. Investigation of all the conditions that could affect the reaction as well as the formed complexes' spectral properties was performed. Upon utilization of the optimum reaction conditions; the spectrofluorimetric method was highly sensitive and showed linearity over the concentration range of 40�700 ng/mL for both ciprofloxacin and norfloxacin with a correlation coefficient of 0.9998 and 0.9997, respectively. The limit of detection was 12.56 ng/mL and 11.44 ng/mL, while the limit of quantification was 38.06 ng/mL and 34.66 ng/mL for ciprofloxacin and norfloxacin, respectively. The developed method was effectively utilized for the estimation of the studied drugs in eye-ear pharmaceutical dosage forms. The achieved results were compared statistically with those of the pharmacopoeial method where no significant difference was perceived concerning both accuracy and precision. 2019 Elsevier B.V.
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 analysis of certain hypoglycemic drugs in the presence of their impurities and degradation products utilizing UPLC-MS/MS
(Royal Society of Chemistry, 2015) Mowaka S.; Mohamed D.; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Cairo; Ein Helwan; 11795; Egypt; Department of Analytical Chemistry; Faculty of Pharmacy; British University in Egypt; El-Sherouk City; 11837; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; 6 October City; 11787; Egypt
A novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of three hypoglycemic drugs namely; sitagliptin (STG), vildagliptin (VLG) and metformin (MET) in the presence of their degradation products and STG related impurities. Chromatographic separation was accomplished on a Hypersil gold 50 mm � 2.1 mm (1.9 ?m) column, using acetonitrile and 0.2% formic acid aqueous solution as the mobile phase with a gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. The selected reaction monitoring (SRM) mode on a triple quadrupole mass spectrometer was used to quantify the drugs utilizing the transitions of 408.12 ? 235.24 (m/z), 304.33 ? 154.32 (m/z), 130.12 ? 71.32 (m/z) and 255.75 ? 166.15 (m/z), for STG, VLG, MET and diphenhydramine (IS), respectively. The method has displayed a lower limit of detection of 1.50 ng mL-1, 1.50 ng mL-1 and 3.00 ng mL-1 for STG, VLG and MET, respectively. The drugs were subjected to forced degradation where it was concluded that STG, VLG and MET were highly susceptible for alkaline stress conditions. In addition, the study of the degradation kinetics of the drugs has proved that the degradation follows a pseudo-first-order reaction. The proposed method was effectively applied for the analysis of laboratory prepared mixtures as well as combined pharmaceutical formulations. No significant difference was found regarding accuracy and precision upon statistical comparison of the obtained results with those of the reported method. Validation was conducted in compliance with the ICH guidelines proving the method to be selective, linear, precise and accurate. The simplicity and sensitivity of this method allows its use in the quality control of the cited drugs. � The Royal Society of Chemistry 2015.
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.
Novel univariate spectrophotometric determination of the recently released solid dosage form comprising dapagliflozin and saxagliptin via factorized response spectra: Assessment of the average content and dosage unit uniformity of tablets
(Elsevier B.V., 2019) Lotfy H.M.; Mohamed D.; Elshahed M.S.; Analytical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr-El Aini Street; Cairo; 11562; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmaceutical Sciences & Pharmaceutical Industries; Future University in Egypt; Cairo; 11835; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Ein Helwan; Cairo; 11795; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; October City 6; 11787; Egypt
Dapagliflozin (DPF) and saxagliptin (SXG) are currently co-formulated in a tablet dosage form which is prescribed to improve glycemic control. The absorption spectra of DPF and SXG were highly overlapped which completely hindered their simultaneous estimation at their ?max 224 nm and 209 nm, respectively. Thus, in this work three smart and simple univariate spectrophotometric methods were originally established and validated for the first time in order to quantitatively estimate DPF and SXG in bulk forms and in combined pharmaceutical formulation without the requirement for any initial separation or treatment. These methods are; factorized zero order method (FZM), factorized derivative method (FDM) and factorized ratio difference method (FRM). These methods were capable of determining DPF and SXG over the range of 2.5�50.0 ?g/mL and 2.5�60.0 ?g/mL, respectively. All the developed methods are based on a novel and unique approach for the spectral recovery of unresolved spectra named; factorized response spectrum (FRS). The exclusivity of the FRS originates from its ability to completely resolve the cited drugs in the mixture and retrieve their original spectra. Selectivity of all proposed methods was assessed by comparing the obtained results of the mixture analysis with those of the pure powdered drugs. Validation of the newly developed methods was applied as recommended by the ICH demonstrating acceptable accuracy and precision. In general, these methods could be effectively employed for the routine quality control investigation of bulk materials and available market formulations. � 2019 Elsevier B.V.
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.
Square wave voltammetric determination of rasagiline mesylate on hanging mercury drop electrode and its application in dosage form and biological fluids
(Institute of Electrical and Electronics Engineers Inc., 2016) Habib I.H.I.; Rizk M.; Mohamed D.; Mowaka S.; El-Eryan R.T.; Microanalytical Chemistry Laboratory; Applied Organic Chemistry Department; National Research Centre; Dokki; Giza; 12622; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; Cairo; 11745; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts; 6 October City; 11787; Egypt; Analytical Chemistry Department; Faculty of Pharmacy; British University in Egypt; El-Sherouk City; 11837; Egypt
A new square wave voltammetric (SWV) method has been developed and validated for the determination of Rasagiline mesylate in bulk, dosage form and human plasma due to a cathodic behaviour of its acetylene group at Hanging Mercury Drop Electrode (HMDE). Many facts such as different supporting electrolytes, scan rate, pulse amplitude, accumulation time and accumulation potential were studied. A good linearity was obtained over a concentration range of (2.8 x10-8 to1.4 x10-7mol L-1) with 99.78% as mean recovery and 1.09%, as the relative standard deviation and limits of detection and quantification were found to be (2.7 x10-9 and 9.24 x1 0-9mol L-1), respectively. The accuracy and precision of the method were within acceptable limits. The method was applied for determining the active ingredients in its tablets with % recoveries � relative standard deviation of 95.46 � 3.7 6 and in spiked human plasma with 94.3 � 2.8 9%, respectively. � 2016 The Authors.
UPLC-MS/MS estimation of paracetamol, pseudoephedrine hydrochloride and brompheniramine maleate in plasma: Application to a pharmacokinetic study on healthy Egyptian volunteers based on ethnic difference
(Elsevier Inc., 2019) Mohamed D.; Hassan O.; Bahnasawy N.; Elnoby A.S.; Mowaka S.; Analytical Chemistry Department; Faculty of Pharmacy; Helwan University; EinHelwan; Cairo 11795; Egypt; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); October City 6; 11787; Egypt; Pharmacology Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); October City 6; 11787; Egypt; Pharmaceutics Department; Faculty of Pharmacy; October University for Modern Sciences and Arts (MSA); October City 6; 11787; Egypt; Clinical Pharmacy Department; Children's Cancer Hospital Egypt (57357)Cairo 11617; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmacy; British University in Egypt; El-Sherouk City; Cairo 11837; Egypt
The current study was focused on establishing a novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method for the quantitative estimation of the co-formulated drugs; paracetamol (PAR), pseudoephedrine hydrochloride (PSD) and brompheniramine maleate (BRP) in human plasma to Egyptian volunteers. Additionally, the study aimed to recognize whether the co-administration of the target drugs to different ethnic population affects their pharmacokinetics. The drugs extraction involved liquid-liquid extraction technique with the aid of ethyl acetate. Reversed phase UPLC separation was accomplished on Agilent Zorbax SB C18 (50 mm � 2.1 mm, 1.8 ?m) column using acetonitrile: 0.1% formic acid (70: 30 v/v) as the mobile phase. Positive electrospray ionization and multiple reaction monitoring were employed. The short analysis time (1 min/sample) was promising as it has allowed the analysis of many human plasma samples per day. The developed method displayed linear ranges of 0.05�20.0 ?g/mL for PAR, 1.0�500.0 ng/mL for PSD and 0.1�50.0 ng/mL for BRP. A detailed validation of the developed method was performed in compliance with the FDA guidelines where all the validation parameters results were satisfactory. The UPLC-MS/MS method was utilized for studying the pharmacokinetics of the three drugs after the oral administration of their combined dosage form to Egyptian healthy volunteers. The pharmacokinetic study was accomplished after agreement of the ethics committee. The achieved pharmacokinetic results by the newly developed method were; Cmax (ng/mL) 8001.77, 127.76, 1.92, tmax (h) 0.75, 1.5, 4.0 and t� (h) 3.3, 4.65, 16.26 for PAR, PSD and BRP, respectively, these results were compared with those obtained from other reported clinical trials done on other races. It was clear that the pharmacokinetic parameters of PAR and PSD were not affected when the same dose was given to volunteers from different ethnic populations. Additionally, the co-administration of PSD and BRP with PAR has not altered the pharmacokinetics of PAR. The pharmacokinetics of PSD when it was co-administered with PAR and BRP was almost similar to that when it was co-administered with benorylate and chlorpheniramine, however, the Cmax of PSD was greatly affected when it was co-administered with caffeine, chlorpheniramine and cloperastine. � 2019 Elsevier B.V.