Login Register Cart 0
Generic placeholder image

Current Pharmaceutical Analysis

Editor-in-Chief

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

Back
Research Article

Development and Validation of a Pre-Column Derivatization HPLC Method for the Assay of Amikacin Sulfate in Pure and Parenteral Dos age Forms

Author(s): Muneeba Usmani, Sofia Ahmed*, Muhammad Ali Sheraz* and Iqbal Ahmad

Volume 15, Issue 5, 2019

Page: [511 - 520] Pages: 10

DOI: 10.2174/1573412914666180314121213

Price: $65

Abstract

Background: Amikacin sulfate (AMK) belongs to the class of aminoglycoside antibiotics. It is effective against the infections caused by Gram-negative and positive bacteria. AMK lacks a chromophore group in its structure and, therefore, it does not absorb light in the 200-800 nm region which makes it a difficult molecule to analyze by UV detector using high performance liquid chromatography (HPLC).

Objective: This study has been carried out to develop and validate a relatively simple, accurate, precise, rapid, economical, and stability-indicating pre-column derivatization HPLC method for the determination of AMK in pure and parenteral dosage forms.

Methods: The stock solution of AMK was derivatized prior to its analysis. The mobile phase used for the analysis was acetonitrile and water in the ratio of 50:50 (v/v) at pH 6.0. The method has been validated according to the guideline of International Council for Harmonization (ICH) and different parameters such as linearity, range, accuracy, precision, sensitivity, robustness, solution stability, specificity and system suitability have been studied. AMK was subjected to stress degradation studies including thermolysis, humidity exposure, acid-base hydrolysis, and oxidation in order to determine the specificity of the test method.

Results: The retention time of AMK has been found to be 4.7 min. The results indicated that the method is linear in the concentration range of 12.5-125% and possesses high accuracy (99.88±0.42%), precision (<1.2%) and robustness (<0.5%). The obtained results are compared statistically with a reference method.

Conclusion: It was observed that the stress degradation studies do not affect the accuracy of the method. Hence the proposed method can be used for the assay of AMK and its parenteral dosage form.

Keywords: Amikacin sulfate, HPLC, pre-column derivatization, validation, parenteral dosage forms, drugs.

« Previous Next »
Graphical Abstract

[1]
Rahman, N.; Azmi, S.N.H.; Wu, H.F. The importance of impurity analysis in pharmaceutical products: an integrated approach. Accredit. Qual. Assur., 2006, 11(1-2), 69-74.
[2]
Alothman, Z.A.; Rahman, N.; Siddiqui, M.R. Review on pharmaceutical impurities, stability studies and degradation products. Rev. Adv. Sci. Eng., 2013, 2(2), 155-166.
[3]
Siddiqui, M.R.; AlOthman, Z.A.; Rahman, N. Analytical techniques in pharmaceutical analysis: a review. Arab. J. Chem., 2017, 10(Suppl. 1), S1409-S1421.
[4]
Sweetman, S.C., Ed.; Martindale: The Complete Drug Reference, 36th ed; Pharmaceutical Press: London, UK, 2009, pp. 200-201.
[5]
Stead, D.A. Current methodologies for the analysis of aminoglycosides. J. Chromatogr. B Biomed. Sci. Appl., 2000, 747(1-2), 69-93.
[6]
Korany, M.A.; Haggag, R.S.; Ragab, M.A.; Elmallah, O.A. Liquid chromatographic determination of amikacinsulphate after pre-column derivatization. J. Chromatogr. Sci., 2014, 52(8), 837-847.
[7]
Lung, K.R.; Kassal, K.R.; Green, J.S.; Hovsepian, P.K. Catalytic precolumn derivatization of amikacin. J. Pharm. Biomed. Anal., 1998, 16(15), 905-910.
[8]
Morovjan, G.; Csokan, P.P.; Nemeth-Konda, L. HPLC determination of colistin and aminoglycoside antibiotics in feeds by post-column derivatization and fluorescence detection. Chromatographia, 1998, 48(1-2), 32-36.
[9]
Ovalles, J.F.; Brunetto Mdel, R.; Gallignani, M. A new method for the analysis of amikacin using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) derivatization and high-performance liquid chromatography with UV-detection. J. Pharm. Biomed. Anal., 2005, 39(1-2), 294-298.
[10]
Nicoli, S.; Santi, P. Assay of amikacin in the skin by high-performance liquid chromatography. J. Pharm. Biomed. Anal., 2006, 41(3), 994-997.
[11]
Al-Majed, A.A. A new LC method for determination of some aminoglycoside antibiotics in dosage forms and human plasma using 7-fluoro-4-nitrobenz-2-oxa-1,3-diazole as a fluorogenic pre-column label. Chromatographia, 2008, 68(11-12), 927-934.
[12]
Chauhan, B.; Jalalpure, S. Analysis of amikacin in human serum by UHPLC with fluorescence detector using chloro-formate reagent with glycine. Pharm. Methods, 2016, 7(2), 99-103.
[13]
Long, Z.; Guo, Z.; Liu, X.; Zhang, Q.; Liu, X.; Jin, Y.; Liang, L.; Li, H.; Wei, J.; Wu, N. A sensitive non-derivatization method for apramycin and impurities analysis using hydrophilic interaction liquid chromatography and charged aerosol detection. Talanta, 2016, 146(1), 423-429.
[14]
Shehzadi, N.; Hussain, K.; Khan, M.T.; Salman, M.; Islam, M.; Khan, H.M. Development of a validated colorimetric assay method for estimation of amikacin sulphate in bulk and injectable dosage form. J. Chem. Soc. Pak., 2016, 38(1), 63-69.
[15]
Soliven, A.; Ahmad, I.A.H.; Tam, J.; Kadrichu, N.; Challoner, P.; Markovich, R.; Blasko, A. A simplified guide for charged aerosol detection of non-chromophoric compounds-Analytical method development and validation for the HPLC assay of aerosol particle size distribution for amikacin. J. Pharm. Biomed. Anal., 2017, 143, 68-76.
[16]
Wong, L.T.; Beaubien, A.R.; Pakuts, A.P. Determination of amikacin in microlitre quantities of biological fluids by high-performance liquid chromatography using 1-fluoro-2,4-dinitrobenzene derivatization. J. Chromatogr. B, 1982, 233(1), 145-154.
[17]
Brajanoski, G.; Hoogmartens, J.; Allegaert, K.; Adams, E. Determination of amikacin in cerebrospinal fluid by high performance liquid chromatography with pulsed electrochemical detection. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 2008, 867(1), 149-152.
[18]
Galanakis, E.G.; Megoulas, N.C.; Solich, P.; Koupparis, M.A. Development and validation of a novel LC non-derivatization method for the determination of amikacin in pharmaceuticals based on evaporative light scattering detection. J. Pharm. Biomed. Anal., 2006, 40(5), 1114-11120.
[19]
Liu, Q.; Li, J.; Song, X.; Zhang, M.; Li, E.; Gao, F.; He, L. Simultaneous determination of aminoglycoside antibiotics in feeds using high performance liquid chromatography with evaporative light scattering detection. RSC Advances, 2017, 7(3), 1251-1259.
[20]
Serrano, J.M.; Silva, M. Determination of amikacin in body fluid by high-performance liquid-chromatography with chemiluminescence detection. J. Chromatogr. B , 2006, 843(1), 20-24.
[21]
Mughal, U.R.; Dayo, A.; Ghoto, M.A.; Madan, L.; Arain, M.I. Quantitative determination of amikacin Sulfate using vanillin from pure and commercial brands available in Pakistan. J. Young Pharm., 2016, 8(1), 28-32.
[22]
British Pharmacopoeia. Monograph on amikacin sulfate. London, UK: Her Majesty’s Stationary Office, 2016, Electronic version
[23]
United States Pharmacopeia 39 / National Formulary 34. Monograph on amikacin sulfate. Rockville, MD, USA: United States Pharmacopeial Convention Inc., 2016, Electronic version.
[24]
Harmonised Tripartite Guideline, I.C.H. Validation of analytical procedures: text and methodology Q2(R1); International Council on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use: Geneva, Switzerland, 2005.
[25]
Swartz, M.E.; Krull, I.S. Handbook of Analytical Validation; CRC Press: Boca Raton, USA, 2012, pp. 61-100.
[26]
Shrivastava, A.; Saxena, P. Validation of analytical methods-methodology and statistics; CBS Publishers & Distributors Pvt. Ltd.: New Delhi, India, 2014, pp. 75-91.
[27]
Lister, A.S. Validation of HPLC methods in pharmaceutical analysis.Handbook of Pharmaceutical Analysis by HPLC; Ahuja, S.; Dong, M.W., Eds.; Elsevier Inc.: Amsterdam, Netherlands, 2005, pp. 191-217.
[28]
Hartmann, C.; Verbeke, J.S.; Enninckx, W.V.; Heyden, Y.V.; Vankeerber, P.; Massrat, D.L. Reappraisal of Hypothesis testing for method validation. Detection of systematic error by comparing the mean of two laboratories. Anal. Chem., 1995, 67(24), 4491-4499.
[29]
Rahman, N.; Khan, S. Circular dichroism spectroscopy: an efficient approach for the quantitation of ampicillin in presence of cloxacillin. Spectrchim. Acta. Part A, 2016, 160, 26-33.
[30]
Rahman, N.; Sameen, S.; Kashif, M. Spectroscopic study on the interaction of haloperidol and 2,4-dinitrophenylhydrazine and its application for the quantification in drug formulations. Anal. Chem. Lett., 2016, 6(6), 874-885.

Rights & Permissions Print Cite
Article Metrics
45
2
© 2024 Bentham Science Publishers | Privacy Policy