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Belal, F.
- Kinetic Spectrophotometric Determination of Isoxsuprine in Dosage forms through Derivatisation with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI)
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1 Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, 35516, Mansoura, EG
1 Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, 35516, Mansoura, EG
Source
Scientia Pharmaceutica, Vol 74, No 3 (2006), Pagination: 99-119Abstract
A simple and sensitive kinetic spectrophotometric method was developed for the determination of isoxsuprine in pharmaceutical preparations. The method is based upon a kinetic investigation of the coupling reaction between isoxsuprine HCl and 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI) in borate buffer of pH 7.8 for a fixed time of 30 min. The absorbance of the yellow coloured product was measured at 395 nm. The absorbance-concentration plot was rectilinear over the range of 2-20 μg mL-1 (r = 0.9994) with minimum detectability of 0.6 μg mL-1 (1.75×10-6M). The different experimental parameters affecting the development and stability of the colour were carefully studied and optimized. The determination of isoxsuprine by the fixed-concentration and rate-constant methods is also feasiKeywords
Kinetic Determination, Isoxsuprine HCl, (NBD-CI), Pharmaceutical Preparations.References
- Reynolds J.E.F., "in Martindale, The Extra Pharmacopoeia", 31st Ed., The Pharmaceutical Press, London 1996, p. 1577,1580.
- Belal F., Al-Badr A.A., Al-Majed A.A. and El-Subbagh H.I., in Analytical Profile of Drug Substances and Excepients, Vol. 26, Brittain, G.H., editor, Academic Press, New York 1999, p. 359-393.
- Reddy M.N., Sankar D.G. and Rao K.V. P. Spectrophotometric determination of isoxsuprine and nyldrine using 1,10 phenanthroline. Indian Drugs. 1998; 35: 163.
- Demir C., Brereton R. G. Mutivariante calibration on designed mixtures of pharmaceuticals. Analyst. 1998; 123: 181-189.
- Daabees H. G. Spectrophotometric determination of isoxsuprine hydrochloride Alex. J. Pharm. Sci. 2001; 15: 25-29.
- Beyene N. W., Vanstaden J. F., Stefan R. I., Aboul-Enein H. Y. Determination of isoxsuprine hydrochloride by sequential injection visible spectrophotometry II Farmaco. 2005; 60: 613-619.
- Belal F., Al-Malaq H. A. and Al-Majed A. A. Voltammetric determination of isoxsuprine and fenoterol in dosage forms and biological fluids through nitrosation J. Pharm. Biomed. Anal. 2000; 23: 1005-1015.
- Belal F., Al-Malaq H.A., Al-Majed A. A., Gadkariem E. A. A stability indicating HPLC method for the determination of isoxsuprine in dosage forms; application to kinetic studies of isoxsuprine. J. Liq. Chromatogr.: Rel. Technol. 2000; 23: 3175-3189.
- Brambilla G., Fiori M., Curiel I., Serpe L.,Gallo P. α1-Acid glycoprotein affinity columns for the clean-up of adrenergic drugs. Analyst. 1998; 123: 2693-2696.
- Kootsra, P. R., Kuijpers C.J.P.F., Wubs K.L. Van Doorn D., Strek S.S., Van Ginkel L. A., Stephany R. W. The analysis of beta-agonists in bovine muscle using molecular imprinted polymers with ion trap LCMS screening. Anal. Chim. Acta. 2005; 529: 75-81.
- Saleh H. M. and At-Ghannam Sh. M. Colourimetric determination of aromatic amino acids. Alex. J. Pharm. Sci. 2000; 14: 25-29.
- El-Enany N. Spectroflurimetric and spectrophotometric determination of gliclazide in pharmaceuticals by derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3 diazole J. Assoc. Off. Anal. Chem. Internationa1. 2003; 86: 209-214.
- El-Enany N., Belal F., Rizk M. Spectrophotometric determination of salbutamol in bulk and dosage forms after derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI). Chem. Anal. 2004; 49: 1-9.
- Al-Majed A.A., Belal F., Abounassif M.A., Khalil N.Y. Fluorimetric determination of Gentamicin in dosage forms and biological fluids through derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI). Microchim. Acta. 2003; 141: 1-6.
- El-Shabrawy Y., Belal F., Sharf El-Din M., Shalan Sh. Spectrophotometric determination of fenoterol hydrobromide in pure and dosage forms. IL Farmaco. 2003; 58: 1033-1038.
- Hassan E.M., Belal F., Al-Deeb O.A. and Khalil N.Y. Spectrofluorimetric determination of vigabatrin and gabapentin in dosage forms and spiked plasma sample through derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI) J. Assoc. Off. Anal. Chem. Internationa1.2001; 84: 1017-1024.
- Espinosa-Mansilla A., Acedovalenzuela M. I., Salinas F. and Canada F. Kinetic determination of ansamicins in pharmaceutical formulations. Anal. Chim. Acta. 1998; 376: 365-375.
- Rizk M., Belal F., lbrahim F., Ahmed S. and El-Enany N. A simple kinetic spectrophotometric method for the determination of certain quinolones in drug formulations. Sci. Pharm. 2000; 68: 173-188.
- Rizk M., Belal F., lbrahim F., Ahmed S. and El-Enany N. A simple kinetic spectrophotometric determination of oxamniquine in formulations and spiked biological fluids. J. Pharm. Biomed. Anal. 2000; 23: 503-513.
- El-Enany N., Belal F and Rizk M. A simple kinetic spectrophotometric method for the determination of isoxuprine in dosage forms. IL Farmaco. 2002; 57: 641-648.
- Miyano, H., Toyo'oka T. and Imai, K. Anal. Chim. Acta. 1985; 170: 81-87.
- Weisberger A., Friess S. L. and Lewis E. S. "Techniques of Organic Chemistry", Vol. III, Part I, Interscience, New York (1953).
- Yatsimirskii, K.B., Kinetic Methods of Analysis", Pergamon Press, Oxford. (1966).
- Laitinen, H.A., Harris W.E., "Chemical Analysis", 2nd ed., McGraw-Hill, New York (1975).
- Chatterjee P.K., Jain C. L., Sethi P.D. Colourimetric determination of isoxsuprine HCI through nitrosation and subsequent chelation Indian Drugs. 1987; 24: 210-213.
- Miller J.C., Miller J.N., editors Statistics for Analytical Chemists, Ellis Horwood Chichester, 1984; 22:82.
- Volpe F., Zintel J., Spiegel D. High-performance liquid chromatographyof two peripheral vasodilators, nylidrin [buphenine] hydrochloride and isoxsuprine hydrochloride in pharmaceutical dosage forms J. Pharm. Sci. 1979;68: 1264-1264.
- Rose, J, Advenced Physico-Chemical Experiments, Pitman, London 1964, p.67.
- Anodic Polaroqraphic Determination of Isradipine in Pharmaceutical Formulations
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Authors
Affiliations
1 Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh-11451, SA
1 Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh-11451, SA
Source
Scientia Pharmaceutica, Vol 72, No 2 (2004), Pagination: 131-142Abstract
The anodic behaviour of isradipine was studied using cyclic voltammetry (CV), direct current (DCt) and differential-pulse (DPP) polarography. Isradipine exhibited well-defined anodic polarographic waves over the pH range of 4-8 in Britton-Robinson buffer (BRb). At pH 6, the analytical pH, the diffusion-current constant (Id) was 2.12 ± 0.42 (n = 4). The oxidation potential is -0.1 0 V vs. Ag/AgCI reference electrode with correlation coefficients of 0.9977 and 0.9948 in the DCt and DPP modes, respectively. The current-concentration plots were rectilinear over the ranges 5-14 μg/ml and 2.4-12 μg/ml using the DCt and DPP modes, respectively. The lower detection limit was 1.12 μg/ml (3.02 × 10-6M) adopting the DPP mode. The proposed method was applied to commercial tablets and capsules, the % recoveries were 100.52 ± 1.267 and 99.4 ± 0.87 (n = 6) for the tablets and 101.3 ± 1.57 and 100.7 ± 2.10 (n = 6) for the capsules adopting both DCt and DPP modes, respectively. The number of electrons involved in the electrode process was accomplished and a proposal of the electrode reaction was presented.Keywords
Isradipine; Anodic Polarography; Dosage Forms.References
- Parfitt K. (Ed.). Martindale, The Complete Drug Reference 33rd Ed. The Pharmaceutical Press, Massachusetts 2002, 916-18.
- The British Pharmacopoeia. The Pharmaceutical Press, London 2000, 768-44.
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- Mieclarek J. Normal-phase TLC separation of enantiomers of 1,4-dihydropyridine derivatives. Drug Dev. Ind. Pharm. 2001; 27: 175-79.
- Abd-Elghany M.F., Abd-Elkawy M., El-Zeany B., Stewart J.T. A stability-indicating high performance liquid chromatographic quantitation of isradipine in the presence of its degradation products. J. Planar Chromatogr. Mod. TLC 1996; 9: 290-92.
- Maurer H.M., Arit J.W. Screening procedure for detection of dihydropyridine calcium channel blockers metabolism in urine as part of a systemic toxicological analysis procedure for acidic compounds by gas-chromatography (GC-MS) after extractive methylation. J. Anal. Toxicol. 1999; 23: 73-80.
- Jean C., Laplanche R. Assay of isradipine and of its major metabolites in biological fluids by capillary gas chromatography and chemical-ionisation mass spectrometry. J. Chromatogr. B. 1988; 72: 61-69.
- Christensen H.R., Angelo H.R., Skajaa K. Determination of isradipine and its metabolite in serum by capillary column gas chromatography with nitrogen selective detection. J. Chromatogr. B. 1992; 112: 161-65.
- Rask H.S., Angelo H.R., Christensen H.R. Enantioselective determination of isradipine in human serum using chiral stationary phase liquid chromatography and gas chromatography with nitrogen selective detection. Chirality, 1998; 10: 808-812.
- Tesarova E., Gilar M., Hobza P., Kabelac M., Deyl Z., Smolkova-Keulemanosova E. Correlation between structure of dihydropyridine calcium antagonists and their retention behaviour and enantioseparation on the β-cyclodextrin stationary phase in HPLC. J. High Reslut. Chromatogr. 1995; 18: 597-601.
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- Takamura K., Kusus F., Abdel-Wadood H., El-Rabbat N., Saleh G., Refaat I. Redox properties of isradipine and its electrochemical detection in the HPLC determination of the compound in human serum. Biomed. Chromatogr. 2000; 14: 453-58.
- Bartlett M.G., Spell J.C, Mathis P.S., Abdel-Ghany M.F., El-Zeany B.E., Abdel-Kawy M., Stewart J.T. Determination of degradation products from calcium-channel blocker isradipine. J. Pharm. Biomed. Anal. 1998; 18: 335-45.
- Abdel-Ghany M.F., El-Zeany B.E., Abdel-Kawy M., Stewart J.T. A stability-indicatng high performance liquid chromatographic assay of isradipine in pharmaceutical preparations. Anal. Lett. 1996; 29: 1157-1165.
- Kuesters E., Dosenbach C., Geber G. Enantiomeric separation of isradipine and related compounds by liquid chromatography with a chiral stationary phase. J. High Resolut. Chromatogr. 1991; 14: 769-771.
- Boutagy J., Ramble F., Dunagan F. Determination of isradipine and the oxidative pyridine metabolite in human plasma by high performance liquid chromatography. J. Chromatogr. 1989; 79: 483-88.
- Al-Suwyeh S.A., Quick, simple and sensitive HPLC method for the determination of isradipine in plasma and its application in pharmacokinetic studies. Anal. Lett. 2002; 35: 1205-1213.
- Belal F., Al-Majed A., Julkhuf S. Voltammetric determination of isradipine in dosage forms and spiked human urine and plasma. J. Pharm. Biomed. Anal. 2003; 31 : 989-98.
- Albini A. and Fasani E., editor, Drugs Photochemistry and Photostability. The Royal Society of Chemistry, Cambridge 1998, 21-23.
- Heyrovsky J., Zuman P. Practical Polarography. Academic Press, New York, 1965, 163.
- Meites L., Israel Y. The calculation of electrochemical kinetic parameters from polarographic current-potential curves. J. Am. Chem. Soc. 1961; 83: 4903-4907.
- Proszt J., Cieleszky V., Gyijrbiro K. Polarographie. Akademiai Kiado, Budapest 1967,385-91.
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- High Performance Liquid Chromatographic Method for the Simultaneous Determination of Labetalol and Hydrochlorothiazide in Tablets and Spiked Human Plasma
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Authors
Affiliations
1 Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh-11451, SA
1 Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh-11451, SA
Source
Scientia Pharmaceutica, Vol 72, No 2 (2004), Pagination: 143-155Abstract
A reversed-phase HPLC method with spectrophotometric detection was developed for the simultaneous determination of labetalol (LBT) and hydrochlorothiazide (HCD). The chromatographic separation was performed using a Microbondapak C18 column (4.6 i.d. × 250 nm) and paracetamol as internal standard. A mobile phase consisting of 0.05 M phosphate buffer/acetonitrile of pH 4 (7:3) at a flow rate of 0.7 ml/min was used. The detection was affected spectrophotometrically at 302 nm. The working concentration range was 0.3-10 μg/ml with detection limits of 0.05 μg/ml for both drugs. The lower quantitation limit was 0.25 μg/ml in the two cases. The method was successfully applied to tablets, the % recoveries were 99.45±0.68 for LBT and 99.79±0.75 for HCD. The method was extended to the in-vitro determination in spiked human plasma. The % recoveries were 91.12±0.33 for LBT and 91.37±0.40 for HCD. The interday and intraday precision and accuracy were evaluated in plasma by calculating the % RSD (n=5) and the % error and were found to be in the ranges of 1.18-4.1% and 0.38-0.36% for both drugs, respectively.References
- Parfitt K, editor. In: Martindale, the Complete Drug Reference, 32nd ed. Massachusetts, 1999, 896.
- British Pharmacopoeia, HMSO, Vol. I and II, London, 2000.
- The United States Pharmacopeia XXIV, the National Formulary, 19. Rockville, Md., USA, 2000.
- Belal F, Al-Shaboury S, Al-Tamrah AS. Spectrofluorometric Determination of Labetalol in Pharmaceutical Preparations and Spiked Human Urine Through the Formation of Coumarin Derivative. J. Pharm. Biomed. Analysis 2002;30:1191-1196.
- Belal F, Al-Shaboury S, Al-Tamrah AS. Spectrophotometric Determination of Labetalol in Pharmaceutical Preparations and Spiked Human Urine. IL-Farmaco 2002;58:293-299.
- Sastry CSP, Krishna DM. Spectrophotometric Methods for the Determination of Labetalol-HCl in Pure and Dosage Forms. Mikrochim. Acta 1996;122:87-93.
- lorio MA, Mazzeo-Frina A, Doldo A. Quantitative Analysis of β-adrenergic Blocking Agents by NMR Spectroscopy. J. Pharm. Biomed. Anal. 1987;5:1-10.
- Witek A, Hopkala H, Matysik G. TLC-Densitometric Determination of Bisoprolol, Labetalol and Propafenone as Dabsyl Derivatives in Pharmaceutical Preparations. Chromatographia 1999;50:41-44.
- Zhao H, Li HZ, Qiu ZY. Separation of Enantiomeric Labetalol by Reversed Phase High-Performance Liquid Chromatography. Sepu. 1999;17:369-371.
- Bazylak G, Aboul-Enein HY. Direct Separation of Labetalol Stereoisomers in a High-Performance Liquid Chromatography System Using Helically Self-Assembled Chelate as Chiral Selector in the Mobile Phase. J. Liq. Chromatogr. Relat. Technol. 1999;22:1171-1192.
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- Abdine HH, El-Yazbi FA, Shaalan RA, Blaih SM. Direct-differential Solubility and Compensatory Derivative Spectrophotometric Methods for Resolving and Subsquently Determining Binary Mixtures of Some Antihypertensive Drugs. STP-Pharm-Sci. 1999;9:587-591.
- Panderi IE. Simultaneous Determination of Benazepril Hydrochloride and Hydrochlorothiazide in Tablets by Second-order Derivative Spectrophotometry. J. Pharm. Biomed. Anal. 1999;21:257-265.
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- Zecevic M, Zivanovic LJ, Agatonovic-Kustrin S, lvanovic D, Maksimovic M,. Statistical Optimiziation of a Reversed-Phase Liquid chromatographic Method for the Analysis of Amiloride and Hydrochlorothiazide in Tablets. J. Pharm. Biomed. Anal. 2000;22:1-6.
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- Derivative UV Spectrophotometric Analysis of some Pharmaceutically Important Halogenated 8-hdroxyquinoline Derivatives via their Pd (II)-complexes
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1 Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, EG
1 Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, EG
Source
Scientia Pharmaceutica, Vol 68, No 3 (2000), Pagination: 297-307Abstract
A derivative UV-spectrophotometric method was developed for the analysis of two halogenated 8-hydroxyquinoline derivatives; iodochlorohyroxyquin (I) (Clioquinol) and di-iodohydroxyquin (II) (iodoquinol). The proposed method depends on the formation of Pd II-ligand complexes in methanol-acetonitrile mixture, which exhibits an UV-spectra with an appreciable value of ε. Zero order (0D), first order (1D) and fourth order (4D) derivative measurements were applied for the quantitative analysis of the drugs. A linear correlation was established between absorbance and concentration for the 0D mode in the range 2-14 μg ml-1 and 2-18 μg ml-1 for (I) and (II) with average % recoveries of 99.83 ± 1.04 and 99.9 ± 10.64 respectively. Also a linear correlation was obtained between the trough of the peak and concentration for 1D mode in the range of 0.16-0.8 μgml-1 for both drugs with average % recoveries of 100.23 ± 1.04 and 100.18 ± 1.14 for (I) and (II) respectively. Besides, the 1D mode was successfully applied for the analysis of binary mixture containing both (II) and metronidazole (III) in tablet formulations. The average % recoveries were 99.42 ± 0.358 and 98.81 ± 0.973 for (II) and (III) respectively. In the 4D mode, a linear correlation was attained between the amplitude of the peak and concentration in the range 0.1-0.8 μg ml-1 for (I) and (II), with average % recoveries of 99.6 ± 0.84 and 100.06 ± 0.98. The limit of detection (LOD) was 2.1ng ml-1 and 2.3ng ml-1 for (I) and (II) respectively. The suggested method was successfully applied for accurate, sensitive and selective analysis of the studied drugs in bulk and single or combined dosage forms with average % recoveries of 99.74 ± 0.480-99.84 ± 0.515 and 99.44 ± 0.71-100.58 ± 1.06 for (1D) and (4D) respectively. The results obtained were favorably compared to those given by a reference method.Keywords
Derivative Spectrophotometry, Halogenated 8-hydroxyquinolines, Pd (II)-complexes, Clioquinol, Iodoquinol, Dosage Forms.References
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- A Simple Kinetic Spectrophotometric Method for the Determination of Certain 4-Quinolones in Drug Formulations
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Authors
Affiliations
1 Department of Analytical, Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, EG
1 Department of Analytical, Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, EG
Source
Scientia Pharmaceutica, Vol 68, No 2 (2000), Pagination: 173-188Abstract
An accurate simple and selective kinetic procedure for the determination of certain 4-quinolones namely, norfloxacin (I), ofloxacin (II), enrofloxacin (III), fleroxacin (IV), ciprofloxacin (V) and pefloxacin (VI) is described. The procedure is based on reacting the studied compounds in acidic media (0.1 M HCL) with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in presence of cerium (IV) ammonium sulphate as an oxidant at room temperature for a fixed time of 20 min. For (I), (III), 12 min for (II) and 30 min for IV , V and VI, then the absorbance of the reaction product is measured at 630 nm. The concentration of the studied compounds is computed using the corresponding calibration curve equation for the fixed-time method. The absorbance-concentrations plot is rectilinear over the range 20-100 ug·ml-1 for (I), 2-20 ug·ml-1 for (II), 10-74 ug·ml-1 for (III), 10-60 ug.ml-1 for IV, 10-50 ug·ml-1 for IV and 8-40 ug·ml-1 for VI. The determination of the studied compounds by the fixed-concentration and rate constant methods is feasible with the calibration equation obtained, but the fixed-time method proved to be more applicable. The procedure was applied successfully to commercial tablets and ampoules and the results obtained were compared statistically with the reference methods.Keywords
Kinetic Determination; 4-Quinolone Antibiotics; 3-Methyl-2-Benzothiazolinone Hydrazone HCL (MBTH); Ce. (IV); Pharmaceutical Analysis.References
- - Martindale, The Extra Pharmacopeia, Reynolds, J.E.F (Ed.), 32nd edn., The Pharmaceutical Press, London, 1999, PP 209.
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