Spectrophotometric and Spectrofluorometric Determination of Heptaminol and mexiletine in Their Dosage Forms

1997 ◽  
Vol 30 (11) ◽  
pp. 2029-2043 ◽  
Author(s):  
Abdel Fattah M. El Walily ◽  
Fawzy A. El-Yazbi ◽  
Saeid F. Belal ◽  
Omayma Abdel-Razak
2007 ◽  
Vol 90 (4) ◽  
pp. 948-956 ◽  
Author(s):  
Nahed El-Enany

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.


2007 ◽  
Vol 90 (2) ◽  
pp. 376-383 ◽  
Author(s):  
Nahed El-Enany

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.


2013 ◽  
Vol 96 (5) ◽  
pp. 968-975 ◽  
Author(s):  
Soad S Abd El-Hay ◽  
Christa L Colyer ◽  
Wafaa S Hassan ◽  
Abdalla Shalaby

Abstract New, sensitive, and selective spectrophotometric and spectrofluorometric methods have been developed for determination of clemastine hydrogen fumarate (Clem), loratadine (Lor), losartan potassium (Los), and ramipril (Ram) in both pure form and pharmaceutical formulations using 4-chloro-7-nitrobenzofurazan (NBD-Cl), which is a highly sensitive chromogenic and fluorogenic reagent. The relation between absorbance at 470, 467, 471, and 469 nm and the concentration was linear over the ranges 5–35, 10–100, 10–90, and 10–120 μg/mL for Clem, Lor, Los, and Ram, respectively. The complexation products were also measured spectrofluorometrically at the emission wavelength 535 nm for Clem, Lor, and Ram and at 538 nm for Los with excitation at 477 and 452 nm for Clem and Lor, respectively, and 460 nm for both Los and Ram. The fluorescence intensity was directly proportional to the drug concentration over the ranges 0.05–0.5, 5–20, 1–6, and 2–15 μg/mL for Clem, Lor, Los, and Ram, respectively. The methods were successfully applied for the determination of the studied drugs in pharmaceutical dosage forms with excellent recovery.


Author(s):  
Hind Hadi ◽  
Gufran Salim

A simple, rapid and sensitive spectrophotmetric method for trace determination of salbutamol (SAL) in aqueous solution and in pharmaceutical preparations is described. The method is based on the diazotization coupling reaction of the intended compound with 4-amino benzoic acid (ABA) in alkaline medium to form an intense orange, water soluble dye that is stable and shows maximum absorption at 410 nm. A graph of absorbance versus concentration indicates that Beer’s law is obeyed over the concentration range of 0.5-30 ppm, with a molar absorbtivity 3.76×104 L.mol-1 .cm-1 depending on the concentration of SAL. The optimum conditions and stability of the colored product have been investigated and the method was applied successfully to the determination of SAL in dosage forms.


Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.


Author(s):  
Sagar Suman Panda ◽  
Ravi Kumar B V V ◽  
D Patanaik

A simple, precise and accurate spectrophotometric method was developed for analysis of the osteoporesis drug alendronate sodium (ALS). The method is based on reaction of the drug with sodium-1,2-naphthoquinone-4-sulphonate (NQS) in presence of alkali to form a brown colored complex giving absorption maximum at 525 nm. The drug obeyed Beer’s law in the range of 5-70 µg/ml with a correlation coefficient of 0.999. The LOD and LOQ values are 1.7 µg/ml and 5.0 µg/ml, respectively. The average recoveries for recovery study were found to be in the range of 99.37%-100.46%. The R.S.D. values for intraday and inter-day precision were found to be 0.48 and 0.62, respectively. The optimized assay conditions were applied successfully for determination of ALS in pharmaceutical dosage forms. No interference was observed from the excipients present in the dosage form. The method is statistically validated as per the ICH requirements.  


2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.


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