Login Register Cart 0
Generic placeholder image

Current Analytical Chemistry

Editor-in-Chief

ISSN (Print): 1573-4110
ISSN (Online): 1875-6727

Back
Journal Home About Journal Editorial Board Journal Insight Current Issue Volumes/Issues
Subscribe
Research Article

Analytical Quality by Design (AQbD) Approach Based HPTLC Method for Quantification of Fisetin with Superior Recovery in Formulations

Author(s): Thasleem Moolakkadath, Mohd Aqil*, Syed Sarim Imam, Abdul Ahad, Arshiya Praveen, Yasmin Sultana, Sayeed Ahmad and Mohd. Mujeeb

Volume 16, Issue 2, 2020

Page: [149 - 157] Pages: 9

DOI: 10.2174/1573411014666180627145031

Price: $65

Abstract

Background: A stability indicating high-performance thin layer chromatography (HPTLC) method was developed for the evaluation of fisetin (FIS) in active pharmaceutical ingredient (API) and marketed capsule formulation in accordance with the ICH guidelines.

Methods: The mobile phase combination toluene: ethyl acetate: formic acid: methanol (3: 5.5: 1: 0.5 v/v/v/v) was optimized with the aid of AQbD approach. The absorbance mode at 254 nm was chosen for densitometric analysis as it gives a compact spot of FIS at Rf value of 0.74.

Results: The R2 value obtained from the linear regression equation of calibration plots made by taking the spot in the concentration range of 100-1400 ng/spot was found to be 0.9993. The observed LOD and LOQ value was found to be 29.8 ng/spot and 98.5 ng/spot, respectively. The exposure of FIS to various stress conditions revealed the fact that the drug is stable in photochemical and dry heat stress conditions without any degradation. The drug-exposed to acidic, alkaline and oxidative stress was found to be degraded into different degradation products with the highest degradation was found in alkaline stress. All degradation products were observed to be fairly separated from well-resolved parent peak of FIS.

Conclusion: The developed HPTLC method have shown well-resolved peaks and also shown good recovery in the compound FIS as well as FIS formulation.

Keywords: Fisetin, HPTLC, recovery, degradation study, AQbD, Active Pharmaceutical Ingredient (API).

« Previous Next »
Graphical Abstract

[1]
Kim, S.C.; Kang, S.H.; Jeong, S.J.; Kim, S.H.; Ko, H.S.; Kim, S.H. Inhibition of c-Jun N-terminal kinase and nuclear factor κ B pathways mediates fisetin-exerted anti-inflammatory activity in lipopolysccharide-treated RAW264.7 cells. Immunopharmacol. Immunotoxicol., 2012, 34(4), 645-650.
[http://dx.doi.org/10.3109/08923973.2011.648270] [PMID: 22239491]
[2]
Gutiérrez-Venegas, G.; Contreras-Sánchez, A.; Ventura-Arroyo, J.A. Anti-inflammatory activity of fisetin in human gingival fibroblasts treated with lipopolysaccharide. J. Asian Nat. Prod. Res., 2014, 16(10), 1009-1017.
[http://dx.doi.org/10.1080/10286020.2014.932351] [PMID: 25263652]
[3]
Pal, H.C.; Athar, M.; Elmets, C.A.; Afaq, F. Fisetin inhibits UVB-induced cutaneous inflammation and activation of PI3K/AKT/NFκB signaling pathways in SKH-1 hairless mice. Photochem. Photobiol., 2015, 91(1), 225-234.
[http://dx.doi.org/10.1111/php.12337] [PMID: 25169110]
[4]
Hanneken, A.; Lin, F.F.; Johnson, J.; Maher, P. Flavonoids protect human retinal pigment epithelial cells from oxidative-stress-induced death. Invest. Ophthalmol. Vis. Sci., 2006, 47(7), 3164-3177.
[http://dx.doi.org/10.1167/iovs.04-1369] [PMID: 16799064]
[5]
Sung, B.; Pandey, M.K.; Aggarwal, B.B. Fisetin, an inhibitor of cyclin-dependent kinase 6, down-regulates nuclear factor-kappaB-regulated cell proliferation, antiapoptotic and metastatic gene products through the suppression of TAK-1 and receptor-interacting protein-regulated IkappaBalpha kinase activation. Mol. Pharmacol., 2007, 71(6), 1703-1714.
[http://dx.doi.org/10.1124/mol.107.034512] [PMID: 17387141]
[6]
Van-Zyl, R.L.; Seatlholo, S.T.; Van-Vuuren, S.F.; Viljoen, A.M. The biological activities of 20 nature identical essential oil constituents. J. Essent. Oil Res., 2006, 18, 129-133.
[http://dx.doi.org/10.1080/10412905.2006.12067134]
[7]
Oyedemi, S.O.; Okoh, A.I.; Mabinya, L.V.; Pirochenva, G.; Afolayan, A.J. The proposed mechanism of bactericidal action of eugenol, a α -terpineol and γ-terpinene against Listeria monocytogenes, Streptococcus pyogenes, Proteus vulgaris and Escherichia coli. Afr. J. Biotechnol., 2009, 8, 1280-1286.
[8]
Peev, C.I.; Vlase, L.; Antal, D.S.; Dehelean, C.A. Szabadai1, Z. Determination of some polyphenolic compounds in buds of alnus and corylus species by HPLC. Chem. Nat. Compd., 2007, 43(3), 259-262.
[http://dx.doi.org/10.1007/s10600-007-0100-7]
[9]
Kubo, I.; Nihei, K.; Shimizu, K. Oxidation products of quercetin catalyzed by mushroom tyrosinase. Bioorg. Med. Chem., 2004, 12(20), 5343-5347.
[http://dx.doi.org/10.1016/j.bmc.2004.07.050] [PMID: 15388161]
[10]
Campillo, N.; Viñas, P.; Férez-Melgarejo, G.; Hernández-Córdoba, M. Dispersive liquid-liquid microextraction for the determination of flavonoid aglycone compounds in honey using liquid chromatography with diode array detection and time-of-flight mass spectrometry. Talanta, 2015, 131, 185-191.
[http://dx.doi.org/10.1016/j.talanta.2014.07.083] [PMID: 25281091]
[11]
Tsimogiannis, D.; Samiotaki, M.; Panayotou, G.; Oreopoulou, V. Characterization of flavonoid subgroups and hydroxy substitution by HPLC-MS/MS. Molecules, 2007, 12(3), 593-606.
[http://dx.doi.org/10.3390/12030593] [PMID: 17851414]
[12]
Parets, L.; Alechaga, E.; Nunez, O.; Javier Saurina, J.; Hernández-Cassou, S.; Puignou, L. Ultrahigh pressure liquid chromatography atmospheric pressure photoionization-tandem mass spectrometry for the determination of polyphenolic profiles in the characterization and classification of cranberry-based pharmaceutical preparations and natural extracts. Anal. Methods, 2016, 8, 4363-4378.
[http://dx.doi.org/10.1039/C6AY00929H]
[13]
Monks, K.; Molnár, I.; Rieger, H.J.; Bogáti, B.; Szabó, E. Quality by Design: Multidimensional exploration of the design space in high performance liquid chromatography method development for better robustness before validation. J. Chromatogr. A, 2012, 1232, 218-230.
[http://dx.doi.org/10.1016/j.chroma.2011.12.041] [PMID: 22226460]
[14]
Rozet, E.; Ziemons, E.; Marini, R.D.; Boulanger, B.; Hubert, P. Quality by design compliant analytical method validation. Anal. Chem., 2012, 84(1), 106-112.
[http://dx.doi.org/10.1021/ac202664s] [PMID: 22107128]
[15]
Mustafa, G.; Ahuja, A.; Baboota, S.; Ali, J. Box-Behnken supported validation of stability-indicating high performance thin-layer chromatography (HPTLC) method: An application in degradation kinetic profiling of ropinirole. Saudi Pharm. J., 2013, 21(1), 93-102.
[http://dx.doi.org/10.1016/j.jsps.2011.11.006] [PMID: 23960823]
[16]
Imam, S.S.; Aqil, M.; Akhtar, M.; Sultana, Y.; Ali, A. Optimization of mobile phase by 32-mixture design for the validation and quantification of risperidone in bulk and pharmaceutical formulations using RP-HPLC. Anal. Methods, 2014, 6, 282-288.
[http://dx.doi.org/10.1039/C3AY41562G]
[17]
Mittal, A.; Imam, S.S.; Parmar, S.; Gilani, S.J.; Taleuzzaman, M. Design of Experiment based Optimized RP-HPLC method for simultaneous estimation of amlodipine and valsartan in bulk and tablet formulations. Austin J. Anal. Pharm. Chem., 2015, 2(6), 1057.
[18]
International Conference on Harmonization (ICH), Validation of Analytical Procedures: Text and Methodology Q2 (R1), 2005 November;

Rights & Permissions Print Cite
Article Metrics
10
© 2024 Bentham Science Publishers | Privacy Policy