Samia Mostafa

Suez Canal University, Al Ismā‘īlīyah, Al Ismā‘īlīyah, Egypt

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Publications (13)16.53 Total impact

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    ABSTRACT: The prerequisites for forensic confirmatory analysis by LC/MS/MS with respect to European Union guidelines are chromatographic separation, a minimum number of two MS/MS transitions to obtain the required identification points and predefined thresholds for the variability of the relative intensities of the MS/MS transitions (MRM transitions) in samples and reference standards. In the present study, a fast, sensitive and robust method to quantify tramadol, chlorpheniramine, dextromethorphan and their major metabolites, O-desmethyltramadol, dsmethyl-chlorpheniramine and dextrophan, respectively, in human plasma using ibuprofen as internal standard (IS) is described. The analytes and the IS were extracted from plasma by a liquid–liquid extraction method using ethyl acetate–diethyl-ether (1:1). Extracted samples were analyzed by ultra-high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Chromatographic separation was performed by pumping the mobile phase containing acetonitrile, water and formic acid (89.2:11.7:0.1) for 2.0 min at a flow rate of 0.25 μL/min into a Hypersil-Gold C18 column, 20 × 2.0 mm (1.9 µm) from Thermoscientific, New York, USA. The calibration curve was linear for the six analytes. The intraday precision (RSD) and accuracy (RE) of the method were 3–9.8 and −1.7–4.5%, respectively. The analytical procedure herein described was used to assess the pharmacokinetics of the analytes in 24 healthy volunteers after a single oral dose containing 50 mg of tramadol hydrochloride, 3 mg chlorpheniramine maleate and 15 mg of dextromethorphan hydrobromide. Copyright © 2014 John Wiley & Sons, Ltd.
    Biomedical Chromatography 10/2014; DOI 10.1002/bmc.3384. · 1.66 Impact Factor
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    ABSTRACT: A high-performance liquid chromatographic method has been developed for the simultaneous analysis of benzonatate (BNZ), diphenhydramine hydrochloride (DPH), guaifenesin (GFN), and phenylephrine hydrochloride (PEP). The separation was achieved using a Thermo C18 reversed-phase column (250 mm × 4.6 mm ID, particle size 5 µ). Dual mode gradient elution was used for the separation and UV detection was carried out at 222 nm. The method was specific and stability indicating as chromatographic conditions provided adequate separation of degradation products. The method showed good linearity in the range of 5–400, 1–120, 3–300, and 2–100 µg/mL for BNZ, DPH, GFN, and PEP, respectively. All the square of the correlation coefficients are 0.999. The degradation products were isolated and identified by NMR, IR, and mass spectroscopy. The proposed method proved to be accurate, precise, selective, and robust. The applicability of the method was evaluated in commercial dosage form analysis as well as in stability studies.
    Journal of Liquid Chromatography &amp Related Technologies 01/2014; 36. · 0.64 Impact Factor
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    ABSTRACT: A series of 3,4-bis-chalcone-N-arylpyrazoles 3a-k was prepared from diacetyl pyrazoles 2a-e. The reaction of 2d and 2e with hydrazine hydrate gave pyrazolo[3,4-d]pyridazine derivatives 4a-b. Furthermore, the reaction of 2a-e with thiosemicarbazide afforded pyrazolo[3,4-d]pyridazine thiocyanate salts 5a-e. The synthesized compounds were subjected to in vivo anti-inflammatory and ulcerogenic activity measurements, in addition to determination of their in vitro COX selectivity, to give a full profile about their anti-inflammatory activities. Compounds 3c, 3f, 3i, and 3e showed significant anti-inflammatory activity among the synthesized compounds. Moreover, docking studies were performed to give an explanation for their anti-inflammatory activity through COX selectivity.
    Archiv der Pharmazie 09/2013; 346(9):688-98. · 1.54 Impact Factor
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    ABSTRACT: A stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed which can separate and accurately quantitate Mebeverine hydrochloride (MEB) and Chlordiazepoxide (CPZ) in commercial tablets. The method has shown adequate separation for MEB and CPZ from their degradation products and main impurities of CPZ whether in pure forms or in commercial tablets. A gradient mobile phase system consisting of (A) water and (B) methanol was used with Phenomenex&® Luna C18 analytical column (250mm x 4.6mm i.d., 5μm ps). Quantitation was achieved with UV detection at 254 nm, based on peak area. MEB and CPZ were subjected to acidic, basic hydrolysis and oxidative degradation to apply stress conditions. The linearity of the proposed method was investigated in the range of 40-130 μg ml-1 (r = 0.9987) for MEB and 8-22 μg ml-1 (r = 0.9991) for CPZ. The limits of detection were 4.77μg ml-1 and 0.71μg ml-1 for MEB and CPZ, respectively. The limits of quantitation were 14.44 μg ml-1 and 2.14 μg ml-1 for MEB and CPZ, respectively. Degradation products of MEB, CPZ and impurities of CPZ did not interfere with the detection of MEB and CPZ. The proposed method can thus be considered as a stability indicating assay.
    Current Analytical Chemistry 01/2013; · 1.19 Impact Factor
  • Journal of chromatographic science 12/2012; · 1.03 Impact Factor
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    ABSTRACT: New, simple, rapid and precise reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of orphenadrine citrate, caffeine and aspirin in presence of aspirin degradation products, orphenadrine citrate and caffeine process related impurities, and excipients. Good resolution and quantization were achieved on reversed-phase column [Phenomenex™ Luna ODS C(18) (25 cm×4.6 mm, 5 µm particles)]. Gradient elution based on; eluant [A]: 0.1% triethylamine in aqueous potassium dihydrogen phosphate buffer (50 mM; pH 3.0), while as, eluant [B]: acetonitrile, at a flow rate of 1.5 mL min(-1). UV quantitation was set at 215 nm. Linearity was exhibited for orphenadrine citrate, caffeine and aspirin within 0.5-150, 0.5-360 or 0.7-301 µg mL(-1) ranges, respectively. Satisfactory validation results were ascertained in terms of low limits of quantiation (6.33×10(-2)-7.94×10(-2)), mean percentage recovery (98.9-101.4%), precision (<2%) and robustness. The proposed method was proved to be specific, robust and accurate for the determination of cited drugs in pharmaceutical preparations in presence of their degradation products.
    Chemical & pharmaceutical bulletin 11/2012; 60(11):1426-36. · 1.70 Impact Factor
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    ABSTRACT: A validated, reliable and accurate reversed-phase high performance liquid chromatographic method using pre-column derivatization was adopted for the simultaneous determination of two ternary mixtures containing omeprazole, tinidazole and doxycycline hyclate or clarithromycin. Separation was achieved on a C18 column, through a gradient elution system using acetonitrile-methanol-water adjusted to pH = 6.60. Drugs were detected at 277 nm over concentration ranges of 1-112, 5-125, 2.5-550 and 2.5-100 µg/mL for omeprazole, tinidazole, doxycycline hyclate and clarithromycin, respectively. This is the first method that has isolated and identified clarithromycin derivative by infrared and mass spectroscopy. This method is the first study for the simultaneous determination of omeprazole, tinidazole, doxycycline hyclate and clarithromycin in combined mixtures and pharmaceutical formulations.
    Journal of chromatographic science 10/2012; · 1.03 Impact Factor
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    ABSTRACT: High-performance liquid chromatography (HPLC) and chemometric methods were applied to the simultaneous determination of the two nonsteroidal antifungal drugs, miconazole (MIC) and nystatin (NYS). The applied chemometric techniques are multivariate methods including classical least squares, principal component regression and partial least squares methods. The ultraviolet (UV) absorption spectra of the standard solutions of the training and validation sets in methanol are recorded in the range of 280-320 nm at 0.2-nm intervals. The HPLC method depends on reversed-phase separation using a C18 column. The mobile phase consists of a mixture of methanol-acetonitrile-ammonium acetate buffer (pH 6; 50 mM) (60:30:10 v/v/v). The UV detector was set at 230 nm. The developed methods were validated and successfully applied to the simultaneous determination of MIC and NYS in their tablets. The assay results obtained using the chemometric methods were statistically compared to those of the HPLC method and good agreement was observed.
    Journal of chromatographic science 08/2012; · 1.03 Impact Factor
  • Analytical Chemistry an Indian Journal. 05/2012;
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    ABSTRACT: An easy, precise and valid extractional-spectrophotometric technique is described for the assessment of metronidazole (MNZ), tinidazole (TNZ), ornidazole (ONZ) and secnidazole (SNZ) in pure state and in their pharmaceutical formulations. The technique includes first the reduction of above cited drugs using HCl and zinc powder, then the formation of intense yellow colored ion-association complex species (1:3 drug/dye) using bromothymol blue (BTB) in a buffered aqueous acidic medium at pH 3-3.50. The colored products are extracted into dichloromethane and quantitatively determined at 416-420 nm. The experimental operating factors influencing the ion-pairs development were studied and optimized to obtain the maximum color intensity. The Beer plots are obeyed in the concentration ranges 2.50-22.50, 2.50-30, 7.50-35 and 5-30 μgml-1 for MNZ, TNZ, ONZ and SNZ, respectively, with correlation coefficients not less than 0.9995. The proposed technique is recommended for the routine quality control analysis of the investigated drugs in commercial tablets with no observed interference from common pharmaceutical adjuvants. Results of such analysis were statistically validated and through recovery studies, showing excellent agreement with those achieved by the reported techniques.
    Pakistan journal of pharmaceutical sciences 01/2012; 25(1):207-17. · 0.95 Impact Factor
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    ABSTRACT: A new series of 1,1'-(5-methyl-1-aryl-1H-pyrazole-3,4-diyl)bis(3-aryl-prop-2-en-1-one) (3a-k) was prepared starting from arylpyrazole derivatives 2a-e. Moreover, the reaction of intermediates 2a,b with hydrazine hydrate afforded pyrazolopyridazines 4a-b while their reaction with thiosemicarbazide gave unexpectedly 3,4,7-trimethyl-2-(4-aryl)-2H-pyrazolo[3,4-d]pyridazin-5-ium thiocyanates 5a-e. Some of novel compounds were investigated for their anti-inflammatory activity as selective COX-2 inhibitor with respect to celecoxib. Some compounds of series 3a-k showed significant results especially 3c compared with celecoxib. In addition, the tested compounds were subjected to docking studies using Molsoft icm pro software to get a deep view about their method of interaction with COX isozymes.
    Conference of Pharmaceutical Sciences (The Pharmaceutical Society of Egypt), Conference center, Cairo University Hostel, Cairo, Egypt; 11/2011
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    ABSTRACT: Two simple, quick and sensitive spectrophotometric methods are described for the determination of enrofloxacin and Pefloxacin. The methods are based on the reaction of these drugs with bromophenol blue (BPB) and methyl orange (MO) in buffered aqueous solution at pH 2.3-2.5 in case of bromophenol blue and at pH 3.6 with MO to give highly coloured complex species, extractable with chloroform. The coloured products are quantitated spectrophotometrically at 420 and 424 nm for BPB and MO, respectively. Optimisation of the different experimental conditions is described. Beer's law is obeyed in the concentration ranges 2-12 and 2-18 microg ml(-1) with BPB and in the ranges 1-12 and 4-40 microg ml(-1)with MO for enrofloxacin and pefloxacin, respectively. The proposed methods are applied for determination of Enroxil oral solution, Peflacine tablets and Peflacine ampoules with mean percentage accuracies 99.5+/-0.99, 99.39+/-1.05 and 100.02+/-0.895, respectively, with BPB and 100.30+/-0.89, 100.25+/-0.98 and 100.20+/-0.72, respectively, with MO.
    Journal of Pharmaceutical and Biomedical Analysis 05/2002; 28(1):173-80. · 2.83 Impact Factor
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    ABSTRACT: A spectrophotometric method was described for the determination of the antibacterial quinolone derivatives, ciprofloxacin, enrofloxacin and pefloxacin through charge transfer complex formation with three different acceptors. Chloranilic acid (CL) was utilized for their determination, forming charge transfer complex with lambdamax 520 nm. The proposed method was applied for determination of Ciprocin tablets, Enroxil oral solution, Peflacin ampoules and Peflacin tablets, with mean percentage accuracies, 99.58+/-1.25,99.94+/-0.96,100.91+/-1.59 and 99.86+/-1.003. Also, tetracyanoethylene (TCNE) was utilized in the determination of the concerned compounds forming charge transfer complexes with maximum absorbances at lambdamax 335 nm for ciprofloxacin and at lambdamax 290 nm for both enrofloxacin and pefloxacin. The procedure was applied for determination of Ciprocin tablets, Enroxil 10% oral solution, Peflacine tablets and Peflacine ampoules with mean percentage accuracies 99.40+/-1.27,99.95+/-0.90,98.98+/-1.565 and 99.88+/-0.998, respectively. Also, 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) was utilized for determination of pefloxacin forming charge transfer complex with maximum absorbance at lambdamax 460 nm. The procedure was applied for determination of peflacine tablets and peflacine ampoules with mean percentage accuracies 100.40+/-0.76 and 99.91+/-0.623, respectively. Statistical analysis of the obtained results showed no significant difference between the proposed method and other official and reported methods as evident from the t-test and variance ratio.
    Journal of Pharmaceutical and Biomedical Analysis 02/2002; 27(1-2):133-42. · 2.83 Impact Factor