Validated Spectrofluorimetric Method for The Determination of Oxymetazoline Hydrochloride via Derivatization with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl)
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Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University, Nasr City, Cairo, EGYPT
Online publication date: 2018-03-20
Publication date: 2018-03-20
Eurasian J Anal Chem 2018;13(4):em25
An accurate and precise spectrofluorimetric method was developed and validated for the determination of non-selective adrenergic drug named; oxymetazoline hydrochloride (OMZ) in its pure form and nasal drops.

Based on nucleophilic substitution reaction of target drug with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) to form a highly fluorescent fluorophore with emission measured at 543 nm after excitation at 400 nm.

Under optimum conditions, the proposed method obeys Beer’s law in the range of (1-12 µg mL-1) and the reaction mechanism was presented.

The method was validated according to ICH guidelines for accuracy, precision and was successfully applied for the determination of the drug in its pure form and nasal drops. The obtained results were statistically compared with those of the reported method and found to be in good agreement.

Windholz M. The Merck Index: an encyclopedia of Chemicals, Drugs and biologicals, tenth ed., Merck & co., Inc., Rahway, NJ, USA 1983. PMid:6361115.
Reynolds JEF. (1996), Martindale, The Extra Pharmacopia, 31st edition, The Royal Pharmaceutical Society, London.
Sankar DG, Sastry CSP, Reddy MN, Aruna M. Spectrophotometric determination of some adrenergic agents using iron(III) and 2, 4, 6-tris (2-pyridyl) -s-triazine. Indian J of pharm sci. 1988;50(3):178-180.
Othman NS, Fathe SA. Indirect Spectrophotometric determination of oxymetazoline hydrochloride. Raf J Sci.2013;24(1):84-96.
Al-Sabha TN, Rasheed B A. Spectrophotometric determination of oxymetazoline hydrochloride based on the oxidation reaction. Jordan J Chem. 2011;6(4):403-411.
Zakaria SA. Spectrophotometric determination of oxymetazoline hydrochloride via oxidative coupling reaction with 4- Amino antipyrine in the presence of potassium periodates. Raf J Sci. 2011;22(4):97-108.
Abdel-Aziz O, El-Kosasy AM, Magdy N, El Zahar NM. Novel spectroscopic methods for determination of cromolyn sodium and oxymetazoline hydrochloride in binary mixture. Spectrochim Acta A. 2014;131:59-66. PMid:24820323.
Hegazy MA, Al-Ghobashy MA, El-Tanany BM, Khattab FI. Spectral resolution and simultaneous determination of oxymetazoline Hydro-chloride and sodium cromoglycate by derivative and ratio‐based Spectrophotometric methods. Eur J chem.2015;6(3):319-324.
Wang NN, Shao Y, Tang YH, Yin H, Wu XZ. Flow-injection chemiluminescence method for the determination of naphazoline hydrochloride and oxymetazoline hydrochloride. Luminescence. 2009;24(3):178–182. PMid:19253271.
El-Tanany BM, Hegazy MA, Al-Ghobashy MA, Khattab FI. Validated chromatographic methods for the simultaneous determination of sodium cromoglycate and oxymetazoline hydrochloride in a combined dosage form. J Advances in Chem. 2015;11(8):3850-3854.
United States Pharmacopoeia 24thed, National formulary 19, Asian edition; Official monographs, 2000.
Hoffmanna TJ, Thompsona RD, Seiferta JR. Determination of the nasal decongestant, oxymetazoline hydrochloride, in pharmaceutical formulations by HPLC. Drug Development and Industrial Pharm. 1989;15(5):743-757.
Shaikh KA, Patil AT. Stability-Indicating HPLC method for the determination of mometasone furoate, oxymetazoline, phenyl ethanol and benzalkonium chloride in nasal spray solution. J of Trace Anal in Food and Drugs 2013;1:14-21.
Sudsakorn S, Kaplan L, Williams DA. Simultaneous determination of triamcinolone acetonide and oxymetazoline hydrochloride in nasal spray formulations by HPLC. J of Pharm and Biomed Anal. 2006;40(5):1273-1280. PMid:16297589.
Stanisz B, Nowiński W. Determination of oxymetazoline hydrochloride and decomposition products by high-performance liquid chromatography. Acta Poloniae Pharmaceutica. 2000;57(6):399-401. PMid:11243242.
ISSA YM, ZAYED SIM. Construction and analytical applications of plastic membrane electrode for oxymetazoline hydrochloride. Anal Sci. 2004;20(2):297-300.
Ghosh PM, Whitehouse MW. 7-Chloro-4-nitrobenzo-2-oxa-1,3-diazole: a new fluorigenic reagent for amino acids and other amines. Biochem. J. 1968;108:155-6. PMid:5657448 PMCid:PMC1198782.
Imai K, Toyo’oka T, Miyano H. Fluorigenic reagents for primary and secondary amines and thiols in high-performance liquid chromatography, A review. Analyst, 1984;109:1365-73.
Moneeb MS. Spectrophotometric and spectrofluorimetric methods for the determination of saxagliptin and vildagliptin in bulk and pharmaceutical preparations. Bulletin of Faculty of Pharmacy, Cairo University. 2013;51(2):139–50.
Darwish IA, Amer SM, Abdine HH, Al-Rayes HL. Spectrofluorimetric Determination of Fluvoxamine in Dosage Forms and Plasma Via Derivatization with 4-Chloro-7-Nitrobenzo-2-Oxa-1,3-Diazole. J. Fluoresc. 2009;19:463-471. PMid:18949539.
Miyano H, Toyo’oka T, Imai K. Further studies on the reaction of amines and proteins with 4-fluoro-7-nitrobenzo-2-oxa-1,3-diazole. Anal. Chim. Acta. 1985;170:81-7.
ICH Harmonized Tripartite Guidelines, Q2 (R1) Validation of Analytical Procedures: Text and Methodology. 2005.