Generic placeholder image

Current Pharmaceutical Analysis

Editor-in-Chief

ISSN (Print): 1573-4129
ISSN (Online): 1875-676X

Research Article

Spectroscopic Fingerprinting of Aminoglycosides and Determination of Neomycin Sulphate Through Oxidative Ion-pair Complex Formation using Ammonium Molybdate

Author(s): Edebi Nicholas Vaikosen*, Benjamin Umar Ebeshi and Chimenem Ruth Worlu

Volume 15, Issue 5, 2019

Page: [487 - 496] Pages: 10

DOI: 10.2174/1573412914666180502124906

Price: $65

Abstract

Background: Aminoglycosides are non-chromophoric antibiotics. The official method of assay in pharmacopoeias is microbiological. Bioassay methods are potency-semi-quantitative, laborious and time-consuming. In contrast, spectrophotometric methods are rapid, convenient, specific, sensitive and selective. The presence of NH2 and -OH functional groups in aminoglycosides makes them susceptible to redox reaction.

Objective: A simple, cheap, quick, accurate and reliable spectrophotometric method for aminoglycoside analysis using neomycin as prototype via oxidation by ammonium molybdate reagent is proposed.

Methods: Four aminoglycosides - amikacin, gentamicin, neomycin and streptomycin, were oxidized using ammonium molybdate (pH<2). These were scanned to obtain visible-spectrophotometric fingerprints. Two assay methods were developed. Method I involved the determination of the drug via the linear proportionality between neomycin and residual molybdate measured at 780nm and 850nm. Method II, an indirect determination using ion-pair reaction of excess molybdate and methyl orange measured at 430nm and 480nm.

Results: All aminoglycosides formed blue complex, with distinct spectra peaks at 500nm, 640nm, 780nm and 850nm.The limit of detection and limit of quantification were from 0.33 to 2.32 μgmL-1 and 1.00 to 7.03 μgm L-1 respectively for both methods. Percentage recoveries ranged from 89.60 and 113.05 %, while precision and accuracy as RSD ranged from 0.23 to 3.55%. The regression coefficient (R2) ranged from 0.9968 to 0.9995. Percentage neomycin in dosage forms ranged from 95.67- 104.16% and 96.04 - 99.46% for methods I and II, respectively.

Conclusion: The methods were successfully applied for neomycin sulphate determination in tablets and drops, therefore aminoglycosides could be assayed via the proposed methods.

Keywords: Antibiotics, aminoglycosides, non-chromophoric, indirect spectrophotometry, oxidative, methyl orange.

Graphical Abstract

[1]
Davies, J.; Wright, G. Bacterial resistance to aminoglycoside antibiotics. Trends Microbiol., 1997, 5, 234-239.
[2]
Jiame, N.D.; William, A.R. Wilson's and Gisvold's text book of organic, medicinal and pharmaceutical chemistry"; 10th ed, 1998. pp. 291, 292
[3]
Cai, Y.Q.; Cai, W.; Cheng, J.; Mou, S.F.; Lu, Y.Q. Comparative study on the analytical performance of three waveforms for the determination of several aminoglycoside antibiotics with high performance liquid chromatography using amperometric detection. Chromatogr. A., 2005, 1085, 124-130.
[4]
McGlinchey, T.A.; Rafter, P.A.; Regan, F.; McMahon, G.P. A review of analytical methods for the determination of aminoglycoside and macrolide residues in food matrices. Anal. Chim. Acta, 2008, 624, 1-15.
[5]
Liu, S.P.; Hu, X.L.; Li, N.B. Resonance rayleigh scattering method for the determination of aminoglycoside antibiotics with trypan blue. Anal. Lett., 2003, 36(13), 2805-2821.
[6]
Isoherranen, N.; Soback, S. Chromatographic methods for analysis of aminoglycoside antibiotics. J. AOAC Int., 1999, 82(5), 1017-1045.
[7]
Stead, D.A. Current methodologies for the analysis of aminoglycosides. J. Chromatogr. B , 2000, 747(1-2), 69-93.
[8]
Li, Q.M.; Gao, L.X. A novel method for the determination of streptomycin using sodium nitroprusside as a chromogenic reagent by spectrophotometry. Anal. Lett., 2008, 41(14), 2595-2607.
[9]
Al-Sabha, T.N. Spectrophotometric determination of amikacin sulphate via charge transfer complex formation reaction using tetracyanoethylene and 2,3-Dichloro-5,6-Dicyano-1,4-Benzoquinone reagents. Arab. J. Sci. Eng., 2010, 35(2A), 27-40.
[10]
David, I.G.; David, V.; Ciuicu, A.A.; Ciobanu, A. Indirect spectrophotometric determination of neomycin based on the reaction with cerium (IV) sulphate. Analele Universităţii din Bucureşti-Chimie (serie nouă), 2010, 19 (1), 61-68
[11]
Omar, M.A.; Nagy, D.M.; Hammad, M.A.; Aly, A.A. Validated spectrophotometric method for determination of certain aminoglycosides in pharmaceutical formulations. J. Appl. Pharm. Sci., 2013, 3(3), 151-161.
[12]
El-Shabrawy, Y. Fluorimetric determination of aminoglycoside antibiotics in pharmaceutical preparations and biological fluids. Spectrosc. Lett., 2002, 35, 99-109.
[13]
Sanchez-Martinez, M.L.; Aguilar-Caballos, M.P.; Gomez-Hens, A. Selective kinetic determination of amikacin in serum using long wavelength fluorimetry. J. Pharm. Biomed. Anal., 2004, 34(5), 1021-1027.
[14]
Hubicka, U.; Krzek, J.; Woltynska, H.; Stachacz, B. Simultaneous identification and quantitative determination of selected aminoglycoside antibiotics by thin-layer chromatography and densitometry. J. AOAC Int., 2009, 92(4), 1068-1075.
[15]
Kaya, S.E.; Filazi, A. Determination of antibiotic residues in milk samples. Kafkas Univ. Vet. Fak. Derg., 2010, 16, S31-S35.
[16]
Sarraguca¸, M.C.; Soares, S.O.; Lopes, J.A. A near-infrared spectroscopy method to determine aminoglycosides in pharmaceutical formulations. Vib. Spectrosc., 2010, 56, 184-192.
[17]
Lin, Y.F.; Wang, Y.C.; Chang, S.Y. Capillary electrophoresis of aminoglycosides with argon-ion laser-induced fluorescence detection. J. Chromatogr. A, 2008, 1188(2), 331-333.
[18]
Yu, C.Z.; He, Y.Z.; Fu, G.N.; Xie, H.Y.; Gan, W.E. Determination of kanamycin A, amikacin and tobramycin residues in milk by capillary zone electrophoresis with post-column derivatization and laser-induced fluorescence detection. J. Chromatogr. B , 2009, 877(3), 333-338.
[19]
Kajita, H.; Akutsu, C.; Hatakeyama, E.; Komukai, T. Simultaneous determination of aminoglycoside antibiotics in milk by liquid chromatography with tandem mass spectrometry. J. Food Hygien. Soc. Japan, 2008, 49(3), 189-195.
[20]
Bohm, D.A.; Stachel, C.S.; Gowik, P. Confirmatory method for the determination of streptomycin in apples by LC-MS/MS. Anal. Chim. Acta, 2010, 672(1-2), 103-106.
[21]
Gremilogianni, A.M.; Megoulas, N.C.; Koupparis, M.A. Hydrophilic interaction vs ion pair liquid chromatography for the determination of streptomycin and dihydrostreptomycin residues in milk based on mass spectrometric detection. J. Chromatogr. A, 2010, 1217(43), 6646-6651.
[22]
Hanko, V.P.; Rohrer, J.S. Determination of neomycin sulfate and impurities using high-performance anion-exchange chromatography with integrated pulsed amperometric detection. J. Pharm. Biomed. Anal., 2007, 43(1), 131-141.
[23]
Sánchez-Martínez, M.L.; Aguilar-Caballos, M.P.; Gómez-Hens, A. Long wavelength homogeneous enzyme immunoassay for the determination of amikacin in water samples. Talanta, 2009, 78(1), 305-309.
[24]
Yamamoto, C.H.; Pinto, T.J. Rapid determination of neomycin by a microbiological agar diffusion assay using triphenyltetrazolium chloride. J. AOAC Int., 1996, 79(2), 434-440.
[25]
The United States Pharcopoeia XXVIIII and NF XXV; American Pharmaceutical Association: Washington, DC, 2007.
[26]
Vishwanathan (2004). Principles of organic chemistry. Jai Sai Pub. pp. 2, 30.
[27]
Adegoke, A.O. Chemical derivatization methodologies for UV-visible spectrophotometric determination of pharmaceuticals. Int. J. Pharm. Sci. Rev. Res., 2012, 14(2), 6-24.
[28]
Darwish, I.A.; Khedr, A.S.; Askal, H.F.; Mahmoud, R.M. Simple and sensitive spectrophotometric methods for determination of amantadine hydrochloride. J. Appl. Spectrosc., 2006, 73(6), 707-712.
[29]
El-Didamoony, A.M.; Ghoneim, A.K.; Amin, A.S.; Telbany, A.M. Spectrophotometric determination of aminoglycoside antibiotics based on their oxidation by potassium permanganate. J. Korean Chem. Soc., 2006, 50, 298-306.
[30]
Basavaiah, K.; Nagegowda, P.; Somashekar, C.B.; Ramakrishna, V. Spectrophotometric and titrimetric determination of ciprofloxacin based on reaction with cerium (IV) sulphate. Sci. Asia, 2006, 32, 403-409.
[31]
Ribeiro, P.R.S.; Pezza, L.; Pezza, H.R. A simple spectrophotometric method for the determination of capopril in pharmaceutical preparations using ammonium molybdate Ecl. Quim. Sào Paulo, 2010, 35 (3): 179-188
[32]
Omara, A.H.; Amin, S.A. Spectrophotometric micro-determination of anti-Parkinsonian and antiviral drug amantadine HCl in pure and in dosage forms. Arab. J. Chem., 2011, 4, 287-292.
[33]
Tao, Y.; Chen, D.; Yu, H.; Huang, L. Liu, Zha.; Cao, X.; Yan, C.; Pan, Y.; Liu, Zhe.; Yuan, Z. Simultaneous determination of 15 aminoglycoside(s) residues in animal derived foods by automated solid-phase extraction and liquid chromatography-tandem mass spectrometry. Food Chem., 2012, 135(2), 676-683.
[34]
Kaufmann, A.; Butcher, P.; Maden, K. Determination of aminoglycoside residues by liquid chromatography and tandem mass spectrometry in a variety of matrices. Anal. Chim. Acta, 2012, 711, 46-53.
[35]
Díez, C.; Guillarme, D.; Sporri, A.S.; Cognard, E.; Ortelli, D.; Edder, P.; Rudaz, S. Aminoglycoside analysis in food of animal origin with a zwitterionic stationary phase and liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta, 2015, 882, 127-139.
[36]
Deck, D.H.; Winston, L.G. Aminoglycosides and Spectinomycin. In: Basic & Clinical Pharmacology. Betram G.K.; Susan B.M.; Anthony, J.T (Eds). McGraw-Hill companies, New York, NY., 2010. pp. 821-822.
[37]
Miller, J.C.; Miller, J.N. Statistics and Chemometrics for Analytical Chemistry, 5th ed; Pearson Education Limited: Harlow, England, 2005.

© 2024 Bentham Science Publishers | Privacy Policy