OPEN ACCESS | PEER-REVIEWED | RESEARCH ARTICLE | DOWNLOAD PDF | VIEW FULL-TEXT PDF | TOTAL VIEWS
Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation
Mohamed Rizk (1) , Ali Kamal Attia (2) , Heba Yosry Mohamed (3,*) , Mona Elshahed (4)
(1) Department of Analytical Chemistry, Faculty of Pharmacy, University of Helwan, Cairo, 11795, Egypt
(2) National Organization for Drug Control and Research (NODCAR), P.O. Box 29, Giza, Egypt
(3) National Organization for Drug Control and Research (NODCAR), P.O. Box 29, Giza, Egypt
(4) Department of Analytical Chemistry, Faculty of Pharmacy, University of Helwan, Cairo, 11795, Egypt
(*) Corresponding Author
Received: 24 Jan 2021 | Revised: 20 Mar 2021 | Accepted: 28 Mar 2021 | Published: 30 Jun 2021 | Issue Date: June 2021
A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.
Links for Article
| | | | | | |
| | | | | | |
| | | |
Article MetricsThis Abstract was viewed 137 times | PDF Article downloaded 22 times
. Madhusudhan, P.; Radhakrishna, M.; Devanna, N. Int. Adv. Res. J. Sci. Eng. Technol. 2015, 2, 95-99.
. Jadhav, S.; Reddy, P.; Narayanan, K.; Bhosale, P. Sci. Pharm. 2017, 85, 25.
. Godasu, S. K.; Sreenivas, S.A. Int. J. Pharm. Sci. Res. 2017, 8, 2223-2232.
. Ayoub, B. M. RSC Adv. 2015, 5, 95703-95709.
. Naazneen, S.; Sridevi, A. Der Pharm. Lett. 2016, 8, 57-65.
. Jyothirmai, N.; Begum, K. M. D.; Supriya, P. J. Atoms Mol. 2016, 6, 977-986.
. Jayalaxmi Rajesh, Dr. T.; Kumar, Dr. G.V. Int. J. Chem. Pharm. Sci. 2016, 4, 634-640.
. Abdel-Ghany, M. F.; Abdel-Aziz, O.; Ayad, M. F.; Tadros, M. M. Acta Chromatogr. 2017, 29, 448-452.
. Srinivasa, R. M.; Anusha, K.; Muneer, S. J. Synth. Nat. Chem. 2017, 2, 1-6.
. Sirigiri, N.; Subramanian, N.; Reddy, G. Saudi J. Med. Pharm. Sci. 2018, 4, 884-896.
. Donepudi, S.; Achanta, S. Int. J. App. Pharm. 2018, 10, 56-61.
. Jagadabi, V.; Nagendra Kumar, P. V.; Pamidi, S.; Ramaprasad, L. A.; Nagaraju, D. Int. Res. J. Pharm. 2018, 9, 192-201.
. Bakshi, A.; Mounika, A.; Bhutada, S.; Raju, Dr. M. B. World J. Pharm. Sci. 2018, 7, 1062-1071.
. Lakshmana, R. A.; Prasanthi, T.; Anusha. E. L. IDMA 2019, 56, 68-71. http://www.indiandrugsonline.org/issuesarticle-details?id=OTM0 (accessed February 01, 2021).
. Vankalapati, K. R.; Alegete, P.; Boodida, S. Biomed. Chromatogr. 2021, 35, e5019.
. Bhole, R. P.; Wankhede, S. B.; Pandey, M. Anal. Chem. Lett. 2017, 7, 76-85.
. Patel, I. M.; Chhalotiya, U. K.; Jani, H. D.; Kansara, D.; Shah, D. A. JPC - J. Planar Chromatogr. - Mod. TLC 2020, 33, 109-118.
. Padmaja, N.; Veerabhadram, G. Der Pharm. Lett. 2015, 7, 306-312.
. Abdel-Ghany, M. F.; Abdel-Aziz, O.; Ayad, M. F.; Tadros, M. M. J. AOAC Int. 2017, 100, 1379-1391.
. Moussa, B. A.; Mahrouse, M. A.; Fawzy, M. G. Spectrochim. Acta A Mol. Biomol. Spectrosc. 2018, 205, 235-242.
. Amin, K. F.; Abdullah, A. M.; Fakhre, N. A. Spectrochim. Acta A Mol. Biomol. Spectrosc. 2019, 222, 117261.
. Elmasry, M. S.; Hasan, M. A.; Hassan, W. S.; Merey, H. A.; Nour, I. M. Spectrochim. Acta A Mol. Biomol. Spectrosc. 2021, 248, 119258.
. Rizk, M.; Attia, A. K.; Mohamed, H. Y.; Elshahed, M. S. Electroanalysis 2020, 32, 1737-1753.
. U. S. Food and Drug Administration, https://www.accessdata.fda.gov/ drugsatfda_docs/nda/2011/201280Orig1s000TOC.cfm (accessed February 01, 2021).
. U. S. Food and Drug Administration, https://www.accessdata.fda.gov/ drugsatfda_docs/nda/2014/204629Orig1s000TOC.cfm (accessed February 01, 2021).
. Abdel-Ghany, M. F.; Abdel-Aziz, O.; Ayad, M. F.; Tadros, M. M. Der Pharma Chem. 2016, 8, 186-189.
. Shah, P. A.; Shrivastav, P. S.; George, A. Microchem. J. 2019, 145, 523-531.
. ICH Guidelines, Stability testing of new drug substances and products Q1A (R2), International Conference on harmonization, Geneva, Switzerland, 2003; pp 1-24.
. ICH Guidelines, In Validation of analytical procedures: text and methodology Q2 (R1), International conference on harmonization, Geneva, Switzerland, 2005; pp 11-12.
. Miller, J. N.; Miller, J. C. Statistics and chemometrics for analytical chemistry, 5th Edition, Pearson Education Limited. Harlow, England. 2005.
. United States Pharmacopeia, USP 39, National Formulary 34. (39th Ed.). Rockville, United States.: United States Pharmacopeial Convention INC. 2017.
How to cite
The other citation formats (EndNote | Reference Manager | ProCite | BibTeX | RefWorks) for this article can be found online at: How to cite item
DOI Link: https://doi.org/10.5155/eurjchem.12.2.168-178.2081
| | | | | | | | |
| | | | | | |
Save to Zotero Save to Mendeley
European Journal of Chemistry 2021, 12(2), 168-178 | doi: https://doi.org/10.5155/eurjchem.12.2.168-178.2081 | Get rights and content
- There are currently no refbacks.
Copyright (c) 2021 Authors
This work is published and licensed by Atlanta Publishing House LLC, Atlanta, GA, USA. The full terms of this license are available at http://www.eurjchem.com/index.php/eurjchem/pages/view/terms and incorporate the Creative Commons Attribution-Non Commercial (CC BY NC) (International, v4.0) License (http://creativecommons.org/licenses/by-nc/4.0). By accessing the work, you hereby accept the Terms. This is an open access article distributed under the terms and conditions of the CC BY NC License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited without any further permission from Atlanta Publishing House LLC (European Journal of Chemistry). No use, distribution or reproduction is permitted which does not comply with these terms. Permissions for commercial use of this work beyond the scope of the License (http://www.eurjchem.com/index.php/eurjchem/pages/view/terms) are administered by Atlanta Publishing House LLC (European Journal of Chemistry).
© Copyright 2010 - 2021 • Atlanta Publishing House LLC • All Right Reserved.
The opinions expressed in all articles published in European Journal of Chemistry are those of the specific author(s), and do not necessarily reflect the views of Atlanta Publishing House LLC, or European Journal of Chemistry, or any of its employees.
Copyright 2010-2021 Atlanta Publishing House LLC. All rights reserved. This site is owned and operated by Atlanta Publishing House LLC whose registered office is 2850 Smith Ridge Trce Peachtree Cor GA 30071-2636, USA. Registered in USA.