scholarly journals Spectrofluorometric Determination of Fluvoxamine in Dosage Forms, Spiked Plasma, and Real Human Plasma by Derivatization with Fluorescamine

2007 ◽  
Vol 90 (2) ◽  
pp. 376-383 ◽  
Author(s):  
Nahed El-Enany
Keyword(s):  
Human Plasma ◽  
Reaction Pathway ◽  
Biological Fluids ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Spectrofluorometric Determination ◽  
Spiked Plasma ◽  
Experimental Parameters ◽  
Good Agreement

Abstract A sensitive, simple, and selective spectrofluorometric method was developed for the determination of fluvoxamine (FXM) in pharmaceutical formulations and biological fluids. The method is based upon the reaction between the drug and fluorescamine in borate buffer of pH 8.0 to yield a highly fluorescent derivative that is measured at 481 nm after excitation at 383 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The method was applied for the determination of the drug over the concentration range of 0.11.1 μg/mL with a detection limit of 0.01 μg/mL (2 10-8 M). The proposed method was successfully applied to the analysis of commercial tablets. The results obtained were in good agreement with those obtained using a reported spectrophotometric method. The method was applied for the determination of FXM in spiked human plasma with recovery (n = 4) of 97.32 1.23%, while that in real human plasma (n = 3) was 90.79 2.73%. A proposal for the reaction pathway is presented.

scholarly journals Micellar Enhanced Spectrofluorometric Determination of Labetalol Through Complexation with Aluminium(III): Application to Dosage Forms and Biological Fluids

2007 ◽  
Vol 90 (4) ◽  
pp. 948-956 ◽  
Author(s):  
Nahed El-Enany
Keyword(s):  
Fluorescence Intensity ◽  
Reaction Pathway ◽  
Biological Fluids ◽  
Sodium Dodecyl ◽  
Dosage Forms ◽  
Spectrofluorometric Determination ◽  
Experimental Parameters ◽  
Fluorescent Products ◽  
Good Agreement

Abstract Two simple, sensitive, and specific spectrofluorometric procedures have been developed for the determination of labetalol (LBT) in pharmaceuticals and biological fluids. LBT was found to react with Al3+ , both in acetate buffer of pH 4.5 (Procedure I) and borate buffer of pH 8.0 (Procedure II), to produce highly fluorescent stable complexes. The fluorescence intensity could be enhanced by the addition of sodium dodecyl sulfate, resulting in 3.5- and 2.7-fold increases in the fluorescence intensity for Procedures I and II, respectively. In both procedures, the fluorescence intensity was measured at 408 nm after excitation at 320 nm. The different experimental parameters affecting the development and stability of the fluorescent products were carefully studied and optimized. The fluorescence intensity-concentration plots were rectilinear over the range of 0.020.1 and 0.010.05 g/mL with a detection limit of 0.003 and 0.001 g/mL for Procedures I and II, respectively. The proposed method was successfully applied to commercial tablets containing LBT. The results were in good agreement with those obtained using a reference spectrofluorometric method. Furthermore, the method was applied for the determination of LBT in spiked human plasma, and the recovery (n = 4) was 93.30 2.62%. A proposal of the reaction pathway was postulated for Procedures I and II, respectively.

scholarly journals Spectrofluorimetric and Spectrophotometric Determination of Gliclazide in Pharmaceuticals by Derivatization with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2003 ◽  
Vol 86 (2) ◽  
pp. 209-214 ◽  
Author(s):  
Nahed El-Enany
Keyword(s):  
Reaction Pathway ◽  
Biological Fluids ◽  
Coupling Reaction ◽  
Pharmaceutical Formulations ◽  
Signal To Noise ◽  
Yellow Fluorescence ◽  
Spectrophotometric Methods ◽  
Experimental Parameters ◽  
Good Agreement

Abstract Accurate, sensitive, and simple spectrophotometric and spectrofluorimetric methods were developed for the determination of gliclazide in pharmaceutical formulations and biological fluids. Both methods are based on a coupling reaction between gliclazide and 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in borate buffer, pH 7.8, in which a yellow reaction product that can be measured spectrophotometrically at 400 nm was developed. The same product exhibited a yellow fluorescence at 470 nm upon excitation at 400 nm. The absorbance–concentration plot was rectilinear over the range of 2–20 μg/mL with minimum detectability [signal-to-noise (S/N) ratio = 2] of 0.2 μg/mL (6.18 × 10−7 M); the fluorescence–concentration plot was rectilinear over the range of 0.2–2.5 μg/mL with minimum detectability (S/N = 2) of 0.02 μg/mL (6.18 × 10−8M). The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. Both methods were successfully applied to the analysis of commercial tablets. The results were in good agreement with those obtained with the official and reference spectrophotometric methods. A proposal of the reaction pathway was presented.

scholarly journals Spectrofluorometric Determination of Olanzapine and Fluphenazine Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Eosin: Application to Stability Studies

2008 ◽  
Vol 91 (6) ◽  
pp. 1309-1317 ◽  
Author(s):  
Fathalla Belal ◽  
Amina El-Brashy ◽  
Nahed El-Enany ◽  
Nihal El-Bahay
Keyword(s):  
Human Plasma ◽  
Reaction Pathway ◽  
Pharmaceutical Preparations ◽  
Stability Studies ◽  
Quenching Effect ◽  
Spectrofluorometric Determination ◽  
The Mean ◽  
Kinetics Of ◽  
Good Agreement

Abstract A simple, rapid, and sensitive spectrofluorometric method has been developed for the determination of olanzapine (OLZ) and fluphenazine hydrochloride (FPZ HCl). The proposed method is based on the quantitative quenching effect of the studied drugs on the native fluorescence of eosin at pH 3.4 and 3.2 for OLZ and FPZ HCl, respectively. The fluorescence was measured at 547 nm after excitation at 323 nm. The fluorescence-concentration plots were rectilinear over the range of 0.051.0 and 0.101.0 g/mL, with lower detection limits of 1.8 103 and 1.2 103 g/mL, for OLZ and FPZ HCl, respectively. The proposed method was successfully applied to the analysis of commercial tablets and ampules containing the drugs, and the results were in good agreement with those obtained with reference methods. The proposed method was further applied to the determination of OLZ in spiked human plasma. The mean recovery was 98.62 0.24 (n 4). The method was also used for stability studies of FPZ HCl upon oxidation with hydrogen peroxide, and the kinetics of the reaction were studied. A proposal for the reaction pathway was postulated.

scholarly journals Spectrofluorimetric Determination of Vigabatrin and Gabapentin in Dosage Forms and Spiked Plasma Samples Through Derivatization with 4-Chloro-7-Nitrobenzo-2-Oxa-1,3-Diazole

2001 ◽  
Vol 84 (4) ◽  
pp. 1017-1024 ◽  
Author(s):  
Ekram M Hassan ◽  
Fathalla Belal ◽  
Omar A Al-Deeb ◽  
Nasr Y Khalil
Keyword(s):  
Reaction Pathway ◽  
Dosage Forms ◽  
Specific Method ◽  
Plasma Samples ◽  
Spiked Plasma ◽  
Highly Sensitive ◽  
Percent Recovery ◽  
Spectrofluorimetric Determination ◽  
Label Claim

Abstract A highly sensitive and specific method is proposed for the determination of vigabatrin (I) and gabapentin (II) in their dosage forms and spiked human plasma. The method is based on coupling the drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in borate buffer at pH 7.1 and measuring the resulting fluorescence at 532 nm after excitation at 465 nm. The fluorescence intensity was a linear function of the concentration of the drugs over the ranges of 1.3–6.5 and 1.7–8.5 μg/mL for I and II, respectively. Minimum detectability values were 0.54 μg/mL (4.2 × 10−6M) and 0.97 μg/mL (5.7 × 10−6M) for I and II, respectively, under the described conditions. The proposed method was successfully applied to the determination of the 2 drugs in their dosage forms, and the percent recoveries ± standard deviation (SD) were 104.53 ± 1.2 and 100.00 ± 1.32 of the label claim for I and II, respectively. The method was further applied to the determination of vigabatrin in spiked plasma samples. The percent recovery ± SD was 101.58 ± 2.68. Interference from endogenous α-amino acids was overcome through selective complexation with freshly prepared Cu(OH)2. The interference likely to be encountered from co-administered drugs, such as carbamazepine, cimetidine, clonazepam, clopazam, phenobarbital, valproic acid, and lamotrigine, was also studied. A reaction pathway is suggested.

scholarly journals Spectrofluorometric Determination of Verapamil Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Organized Media: Application to Stability Studies

2006 ◽  
Vol 89 (6) ◽  
pp. 1565-1572 ◽  
Author(s):  
Mohamed Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelsalam
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Stability Studies ◽  
Verapamil Hydrochloride ◽  
Spiked Human Plasma

Abstract A highly sensitive spectrofluorometric method was developed for the determination of verapamil hydrochloride (VP HCl) in pharmaceutical formulations and biological fluids. The proposed method is based on investigation of the fluorescence spectral behavior of VP HCl in micellar systems, such as sodium dodecyl sulfate (SDS) and β-cyclodextrin (β-CD). In aqueous solutions of borate buffer of pH 9 and 8.5, VP HCl was well incorporated into SDS and β-CD, respectively, with enhancement of its native fluorescence. The fluorescence was measured at 318 nm after excitation at 231 nm. The fluorescence intensity enhancements were 183 and 107% in SDS and in β-CD, respectively. The fluorescence-concentration plots were rectilinear over the range of 0.020.2 and 0.020.25 μg/mL, with lower detection limits of 5.58 × 103 and 3.62 × 103 μg/mL in SDS and β-CD, respectively. The method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained with the official method. The method was further applied to the determination of VP HCl in real and spiked human plasma. The mean % recoveries in the case of spiked human plasma (n 4) was 92.59 3.11 and 88.35 2.55 using SDS and β-CD, respectively, while that in real human plasma (n 3) was 90.17 6.93 and 89.17 6.50 using SDS and β-CD, respectively. The application of the method was extended to the stability studies of VP HCl after exposureto ultraviolet radiation and upon oxidation with hydrogen peroxide.

scholarly journals Spectrofluorometric Determination of Ketorolac Tromethamine Via Its Oxidation with Cerium(IV) in Pharmaceutical Preparations and Biological Fluids

2007 ◽  
Vol 90 (4) ◽  
pp. 941-947 ◽  
Author(s):  
Manal Eid ◽  
Amina El-Brashy ◽  
Fatma Aly ◽  
Wael Talaat
Keyword(s):  
Biological Fluids ◽  
Sulfuric Acid Concentration ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Eye Drops ◽  
Ketorolac Tromethamine ◽  
Accuracy And Precision ◽  
Spectrofluorometric Determination

Abstract A simple and sensitive fluorometric method for determination of ketorolac tromethamine was studied. The method depends on oxidation of the drug with cerium(IV) and subsequent monitoring of the fluorescence of the induced cerium(III) at em 365 nm after excitation at 255 nm. Different variables affecting the reaction conditions, such as the concentrations of cerium(IV), sulfuric acid concentration, reaction time, and temperature, were carefully studied and optimized. Under the optimum conditions, a linear relationship was found between the relative fluorescence intensity and the concentration of the investigated drug in the range of 0.10.8 g/mL. No interferences could be observed from the excipients commonly present in dosage forms. The proposed method was successfully applied to the analysis of the investigated drug in its pure form, pharmaceutical preparations, and biological fluids with good accuracy and precision. The recoveries for pharmaceutical formulations ranged from 99.8101.0 0.6% for tablets, 98.5101.0 1.0% for ampoules, and 99.0100.5 0.7% for eye drops. The results obtained by the proposed method were satisfactory compared with those obtained by the official method. The recoveries for biological fluids were 99.1100.4 0.7 and 99.0100.0 0.5% for plasma and urine, respectively.

scholarly journals Second Derivative Synchronous Fluorescence Spectroscopy for the Simultaneous Determination of Metoclopramide and Pyridoxine in Syrup and Human Plasma

2008 ◽  
Vol 91 (3) ◽  
pp. 542-550 ◽  
Author(s):  
Nahed El-Enany
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
High Sensitivity ◽  
Second Derivative ◽  
Native Fluorescence ◽  
Highly Sensitive ◽  
Experimental Parameters ◽  
The Mean ◽  
Good Agreement

Abstract A rapid, simple, and highly sensitive second derivative synchronous fluorometric method has been developed for the simultaneous determination of metoclopramide (MT) and pyridoxine (PY) in a binary mixture. The method is based on measurement of the native fluorescence of these drugs at = 80 nm in methanol. The different experimental parameters affecting the native fluorescence of the drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the ranges of 0.020.4 and 0.12 g/mL for MT and PY, respectively. The limits of detection were 0.003 and 0.007 g/mL and the limits of quantification were 0.008 and 0.02 g/mL for MT and PY, respectively. The proposed method was successfully applied to the determination of MT and PY in synthetic mixtures and in commercial syrup. The results were in good agreement with those obtained with a reported method. The high sensitivity attained by the proposed method allowed the determination of MT in spiked and real human plasma samples. The mean percent recoveries of MT from spiked and real human plasma (n = 3) were 93.72 3.15 and 89.72 2.19, respectively.

scholarly journals SPECTROPHOTOMETRIC DETERMINATION OF PROPRANOLOL HYDROCHLORIDE AND METOPROLOL TARTRATE IN PHARMACEUTICAL DOSAGE FORMS, SPIKED WATER AND BIOLOGICAL FLUIDS

2018 ◽  
Vol 10 (2) ◽  
pp. 107
Author(s):  
D. K. Sharma ◽  
Jasvir Singh ◽  
Pushap Raj
Keyword(s):  
Water Samples ◽  
Carbon Disulphide ◽  
Biological Fluids ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Metoprolol Tartrate ◽  
Propranolol Hydrochloride ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard

Objective: A new spectrophotometric method for the determination of propranolol hydrochloride (PRO) and metoprolol tartrate (MTP), beta blocker drugs, has been developed for their analysis in pharmaceutical dosage forms for the purpose of quality control and water samples for monitoring impact on environmental water quality of natural sources and in biological fluids for ascertaining their physiological performance.Methods: The method is based on the derivatization of the amino function present in these drugs to the corresponding yellow copper (I) drug dithiocarbamate derivative through reaction with carbon disulphide, pyridine and copper (I) perchlorate in aqueous acetonitrile and measuring absorbance at 406 nm for propranolol and 400 nm for metoprolol. The different experimental parameters affecting the development and stability of the colour were carefully studied and optimized.Results: The Beer’s law is obeyed in the range of 1.0-40.0 μg/ml of each drug solution with a correlation coefficient 0.999. The maximum relative standard deviations (RSDs) in the analysis of pure PRO and MTP were 1.01 and 1.52 % respectively. The recoveries of the drugs from pharmaceutical formulations, spiked water samples and biological fluids were in the range 98.0-100.5 % with RSDs in the range 0.23-1.94% indicating good accuracy and precision of the method.Conclusion: The instantaneous development of colour and its stability, well-established stoichiometry of the reaction and above simplicity and rapidity of procedures are some special attributes of the proposed method.

scholarly journals A Reversed-Phase High-Performance Liquid Chromatographic Method for the Determination of Zafirlukast in Pharmaceutical Formulations and Human Plasma

2006 ◽  
Vol 89 (6) ◽  
pp. 1557-1564 ◽  
Author(s):  
İncilay SÜsÜl ◽  
Sacide AltinÖz
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Chromatographic Method ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Spiked Plasma ◽  
Liquid Chromatographic

Abstract Zafirlukast (ZAF) is a leukotriene receptor antagonist used in the treatment of chronic asthma. In this study, a simple and sensitive reversed-phase, high-performance liquid chromatographic method was developed for the determination of ZAF in pharmaceutical formulations and human plasma. Piribedil was used as an internal standard. Analysis was carried out on a Nucleosil C18 100 Å(150 × mm 4.6 mm id, 5 ωm) column with acetonitrilepH 3.0 acetate buffer (70 30, v/v) as the mobile phase at a flow rate of 0.8 mL/min. The peak was detected by an ultraviolet detector set at a wavelength of 240 nm. The retention times were about 3.9 min for piribedil and 5.8 min for ZAF. The developed method was applied to the determination of ZAF in its pharmaceutical formulation and spiked human plasma. For quantification of ZAF in spiked plasma, proteins were precipitated with ethanol before chromatographic analysis. The calibration range was linear from 49.69437.50 ng/mL in spiked plasma. The absolute recovery from spiked plasma was 98.73 ± 0.42% at a concentration of 254.78 ng/mL of ZAF. No endogenous substances from plasma were found to interfere.

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