Horria A. Mohamed

Antibacterial effect of various shapes of silver nanoparticles monitored by SERS

A comparative evaluation of antimicrobial effect of synthesized silver nanoparticles (AgNPs) of different shapes using different methods was performed. Spherical, triangular and hexagonal AgNPs with an average size of 40 nm were chemically prepared and characterized by transmission electron microscope (TEM) and UV-visible spectroscopy. The antimicrobial effect of these different AgNPs against the gram negative bacterium Escherichia coli (E. coli) was studied by surface enhanced Raman spectroscopy (SERS), the evaluation of growth curves and inhibition zones. SERS proved to be sensitive to monitor the changes that occurred in the bacterial cells upon interaction with AgNPs, which qualitatively compared well with the data provided by the reference methods. However, as SERS is already sensitive to initial changes in the chemistry of bacteria due to the antibacterial effect of the AgNPs, fast and detailed information is provided by SERS as opposed to the classical reference methods based on the evaluation of growth curves and inhibition zones. The results of this work also demonstrate that hexagonal AgNPs display the highest antibacterial effect when compared to other NPs shapes, with triangular AgNPs exhibiting no antibacterial effect under the adopted conditions.

Potentiometric and spectrofluorimetric studies on complexation of tenoxicam with some metal ions

The interaction of tenoxicam with six metal ions, viz. Fe(III), Bi(III), Sb(III), Cr(III), Cd(II) and Al(III) was studied using potentiometric and fluorimetric methods. In the potentiometric method the ionization constant of the ligand and stability constants of the complexes formed have been tabulated at 25+/-0.1 degrees C, ionic strength of NaNO3 in 50% (v/v) aqueous acetonitrile solution was 0.05 mol x dm(-3). Complexes of 1:1 and/or 1:2 and/or 1:3 metal to ligand ratios are formed. The fluorescence of tenoxicam in the presence and absence of the metal ions was studied. The drug can be determined fluorimetrically in 0.5 M HNO3 at an emission wavelength of 450 nm (excitation at 350 nm). The linear range is 0.040-0.2 microg/ml in the absence of Al(III) and 0.016-0.1 microg/ml in the presence of Al(III). Tenoxicam was determined by the proposed method in tablet, suppository and injection. The recovery percent ranged from 98.16 to 102.22%. The effect of 2-aminopyridine on the recovery of tenoxicam was also investigated.

Spectrophotometric determination of some dibenzazepines

Abstract Simple and sensitive method is proposed for determination of four di-benzazepine derivatives. The method is based on the oxidation of dibenzazepines by potassium dichromate in acid medium. The reaction was followed spectrophoto-metrically by measuring the rate of change in absorbance of the coloured products at 670 nm. Linear calibration graphs from 5-50 μg/ml of the final solutions are obtained for all the studied drugs. The method has been successfully applied to the determination of dibenzazepines in some commercial and laboratory prepared tablets. The results were compared statistically with those obtained by official procedures.

Determination of memantine in rat plasma by HPLC-fluorescence method and its application to study of the pharmacokinetic interaction between memantine and methazolamide.

A sensitive high-performance liquid chromatographic method with fluorescence detection was developed to determine memantine (MT) in rat plasma. The method consists of pre-column labeling of MT with 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) and a clean-up step with solid-phase extraction. A good separation of DIB-MT was achieved within 12 min on an octadecylsilica (ODS) column (150 × 4.6 mm i.d.; 5 µm) with a mobile phase of acetonitrile-water (70:30, v/v). The calibration curve prepared with fluoxetine as an internal standard showed good linearity in the range of 10-400 ng/mL (r = .999). The limits of detection and quantitation at signal-to-noise ratios of 3 and 10 were 2.0 and 6.6 ng/mL, respectively. The method was shown to be reliable with precisions of <5% for intra-day and <9% for inter-day as relative standard deviation. The fluorescence property and reaction yield of authentic DIB-MT were also examined. The proposed method was successfully applied to study the pharmacokinetic interaction between MT and methazolamide.

Simultaneous determination of free and bound adriamycin, adriamycinol, adriamycinone and duanorubicin in plasma using column-switching technique and protein-coated pre-columns☆

Adriamycin, adriamycinol, adriamycinone and duanorubicin were simultaneously determined by the development of an on-line plasma clean-up system. A short protein-coated Lichrosorb, RP-8, RP-2, CN and muBondapak phenyl as well as ODS silica have been examined for their performance as pre-columns. The drugs and metabolites were separated from weakly retained plasma components through two steps; phosphate buffer saline, pH 7.4 and 15% acetonitrile in 0.1 M sodium dihydrogen phosphate, pH 3. The chromatographic conditions were: ODS/TM column, flow rate 1 ml/min, 35% acctonitrile in 0.1 M sodium dihydrogen phosphate (pH 3) containing 0.3% heptafluorobutyric acid as mobile phase. The detection was carried out using fluorescence monitor operated at an emission 555 nm and excitation 460 nm. Good resolution was obtained within 13 min. This method is reproducible for analysis of drugs and metabolites (99.3-100.1%, CV < 2%) in plasma.

Utility of surface enhanced Raman spectroscopy (SERS) for elucidation and simultaneous determination of some penicillins and penicilloic acid using hydroxylamine silver nanoparticles.

Elucidation and quantitative determination of some of commonly used penicillins (ampicillin, penicillin G and carbenicillin) in the presence of their main degradation product (penicilloic acid) were developed. Forced acidic and basic degradation processes were applied at different time intervals. The formed degradation products were elucidated and quantified using surface enhanced Raman spectroscopy (SERS). Silver nanoparticles (AgNPs) prepared by reduction of silver nitrate using hydroxylamine-HCl in alkaline medium were used as SERS substrate. The results obtained in SERS were confirmed by the application of LC/MS method. The concentration range was 100-600 ng/ml in case of the studied penicillins and 100-700 ng/ml in case of penicilloic acid. An excellent correlation coefficient was found in case of ampicillin (r=0.9993) and in the case of penicilloic acid (r=0.9997). Validation procedures were carried out including precision, robustness and accuracy by comparing F- and t-values of both the proposed and reported methods.

Utility of quercetin for determination of some tertiary amine and quaternary ammonium salts

A simple and sensitive spectrophotometric method for the assay of eight drugs containing quaternary ammonium or tertiary amine moieties is described. The method is based on the interaction of these drugs with quercetin after its oxidation with N-bromosuccinimide (as counter ion) to give highly colored ion-pairing complexes extractable with organic solvents. The absorbances of the colored complexes are measured in the range of 528-560 nm. Beers law is obeyed for the studied drugs in the range 5-30 mug ml(-1). The method is successfully applied to the analysis of the studied drugs in commercial dosage forms.

Highly reproducible SERS detection in sequential injection analysis: Real time preparation and application of photo-reduced silver substrate in a moving flow-cell

This paper reports an improved way for performing highly reproducible surface enhanced Raman scattering of different analytes using an automated flow system. The method uses a confocal Raman microscope to prepare SERS active silver spots on the window of a flow cell by photo-reduction of silver nitrate in the presence of citrate. Placement of the flow cell on an automated x and y stages of the Raman microscope allows to prepare a fresh spot for every new measurement. This procedure thus efficiently avoids any carry over effects which might result from adsorption of the analyte on the SERS active material and enables highly reproducible SERS measurements. For reproducible liquid handling the used sequential injection analysis system as well as the Raman microscope was operated by the flexible LabVIEW based software ATLAS developed in our group. Quantitative aspects were investigated using Cu(PAR)2 as a model analyte. Concentration down to 5×10(-6) M provided clear SERS spectra, a linear concentration dependence of the SERS intensities at 1333 cm(-1) was obtained from 5×10(-5) to 1×10(-3) with a correlation coefficient r=0.999. The coefficient of variation of the method Vxo was found to be 5.6% and the calculated limit of detection 1.7×10(-5) M. The results demonstrate the potential of SERS spectroscopy to be used as a molecular specific detector in aqueous flow systems.

Use of 7,7,8,8-tetracyanoquinodimethane for spectrophotometric determination of certain local anaesthetics and procainamide hydrochloride

A simple and rapid spectrophotometric procedure has been developed for the determination of four local anaesthetics containing a free primary amine moiety and of procainamide hydrochloride as the drug substances and in dosage forms. The method is based on the reaction of the drug with 7,7,8,8-tetracyanoquinodimethane in alkaline solution to produce yellow products. The chromogen was measured at 473 nm. The effects of several variables on colour development were established. Jobs plots of absorbance versus molar ratio of drug to reagent indicated a 1:1 ratio for all the drugs studied. Results of the analysis of drug substances and their dosage forms by the proposed method are in good agreement with those obtained by the USP XX method.

Effect of cyclodextrins on the stability of adriamycin, adriamycinol, adriamycinone and daunomycin

The stability of adriamycin (ADR), adriamycinol, adriamycinone (ADR-ONE) and daunomycin in the presence of alpha-, beta- and gamma-cyclodextrins (CDs) was studied using high-performance liquid chromatography. It was found that alpha-CD did not affect the degradation of tested compounds, beta-CD caused a little effect and gamma-CD resulted in pronounced stabilizing effect. The formation of complexes between ADR and ADR-ONE with CDs was monitored by fluorescence spectroscopy. The fluorescence spectrum of ADR-gamma-CD complex had an activation maximum at 460 nm, emission maximum at 555 nm and a shoulder at 585 nm. A similar finding was observed in case of alpha-CD. In case of beta-CD, the fluorescence intensity at 580 nm peak enhanced less than in case of gamma-CD. With ADR-ONE, alpha-CD did not cause any significant change compared with the spectrum of free molecule. On the other hand, it was noticed that, the fluorescence spectra of ADR-ONE with both beta- and gamma-CD were the same but showed a significant difference to the spectrum of free molecule, especially the molar fluorescence of the 585 nm emission peak.