Abstract
Objective: An impressionable, discriminatory and precise stability indicating high
performance thin layer chromatographic method has been developed and validated for the estimation
of Enzalutamide in bulk and synthetic mixture.
Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the
stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of
enzalutamide was detected to be 0. 39 ± 0. 005 and the densitometric analysis was carried out in
absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a
virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band.
Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and
27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry
heat degradation and photolytic degradation. The degraded product peaks were well resolved from
the pure drug peak with substantial difference in their Rf values.
Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was
validated with respect to linearity, accuracy, precision and robustness. The method was successfully
applied to the estimation of enzalutamide in synthetic mixture.
Keywords:
Enzalutamide, forced degradation, HPTLC, validation, anti-cancer drug, TLC method.
Graphical Abstract
[1]
Shethi PD. InHPTLC–High Performance ThinLayer Chromatography ; 1st Ed; CBS Publishers, New Delhi, (1996) 1- 68.
[2]
Bailey LC. In Chromatography in the scienceand practice of pharmacy (Remington). 14th ed. Mark Publishing Company Pennsylvania 1995; pp. 534-8.
[3]
Sethi PD. InHPTLC: Quantitative Analysis of Pharmaceutical formulation; 1st. 1996; pp. 162-5.
[4]
Stahl E. InThin Layer Chromatography: A Laboratory Handbook; 2 nd Edn; SpringerInternational, Berlin 1965; 1-30.
[6]
Astellas, “NICE Final Appraisal Determination (FDA) recommends use of prostate cancer treatment XTANDI prior to chemotherapy”. 2015, https://www.astellas.comenirpdfpress release151221.pdf.
[8]
Zamir GK, Swetal SP, Prashant KD, Pravin OP. Validated UV spectroscopic methods for determination of enzalutamide in pure and pharmaceutical dosage form. Ana Chem Indian J 2016; 16(15): 1-8.
[9]
Khan ZG, Patil SS, Deshmukh PK, Patil PO. Validated rp-hplc method for determination of enzalutamide in bulk drug and pharmaceutical dosage form. Indian Drugs 2016; 53(11): 46-9.
[10]
Song JH, Kim TH, Jung JW, et al. Quantitative determination of enzalutamide, an anti-prostate cancer drug, in rat plasma using liquid chromatography-tandem mass spectrometry, and its application to a pharmacokinetic study. Biomed Chromatogr 2014; 28(8): 1112-7.
[11]
Usmangani KC, Kashyap KB, Dimal AS, et al. Estimation of centrally acting muscle relaxant drug tolperisone hydrochloride using HPTLC method. World J Anal Chem 2013; 1(1): 1-7.
[12]
Dimal AS, Dixita JS, Chirag DN, Usman KC, Kashyap KB. Development and validation of HPTLC method for estimation of ibuprofen and famotidine in pharmaceutical dosage form. J Liq Chromatogr Relat Technol 2014; 37(7): 941-50.
[13]
Sarnjitsinh Monika Bakshi. Pharma. Technology On-line 2000; 2000: 1-14.
[14]
Attimarad M1. Ahmed KK, Aldhubaib BE, Harsha S. High-performance thin layer chromatography: A powerful analytical technique in pharmaceutical drug discovery. Pharm Methods 2011; 2(2): 71-5.
[15]
International Conference on Harmonization (ICH); Validation of analytical procedures: Methodology (Q2R1); Food and Drug Administration, USA. 2005.
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