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Stability-Indicating Method of Entacapone-Related Substances Using UPLC in Finished Dosage Form


Affiliations
1 Department of Chemistry, GITAM University, Hyderabad 502 329, India
 

A rapid, specific, sensitive and robust method for entacapone-related substances in carbidopa, entacapone and levodopa film-coated tablet was developed using ACQUITY UPLC with BEH C18 column. Mobile phase (A), i.e. 0.1% orthophosphoric acid and mobile phase (B), i.e. acetonitrile with water in the ratio 75 : 25 (v/v) with gradient method were employed. The method was evaluated for identification of process impurities and unknown impurities. It has been validated according to ICH (Q2) R1 guidelines. The values of LOD and LOQ for impurity and entacapone were found to be 0.01% and 0.03% respectively. Degradation studies were carried out in peroxide, acid, alkali conditions and contribution to mass balance was established. It was stable under heat, light-exposed and humid conditions.

Keywords

Entacapone-Related Substances, Dosage Form, Force Degradation Study, Liquid Chromatography.
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  • Comtan200mgtabIUSPIRx10_2011highlighted – Novartis; https://www.pharma.us.novartis.com/product/pi/pdf/comtan.pdf

  • www.accessdata.fda.gov/frugsatfda_docs/nda/2003/21-485_ STALEVO_Chemr.pdf

  • www.ema.europa.eu/docs/en_GB/document_library/.../WC5001026.pdf

  • Shashikant, A., Sunanda, A., Sachin, Z., Padma, T., Rajesh, H. and Aparna, D., Assay method of active pharmaceutical liquid chromatographic technique. Int. J. Sci. Eng. Res., 2014, 5(2), 462–466.

  • Prafullachandra, T., Vinayak, S. M., Pai, N. R., Chandrabhanu, M. and Smruti, T., Estimation of entacapone tablets by reverse phase high performance liquid chromatography method. J. Biosci. Discov., 2011, 2(3), 294–298.

  • Kumaraswamy, G., Kumar, M. R. J. and Seshagirirao, N., A validated RP-HPLC method for the simultaneous determination of levodopa, carbidopa and entacapone in tablet dosage forms. World J. Pharm. Res., 2014, 3(10), 1684–1690.

  • Rajkumar, D., Ravi, S., Subburaju, T., Revathi, H., Arul, C. and Ganapathirao, N., Development and validation of stabilityindicating RP-HPLC assay method for entacapone in entacapone tablets. Int. J. Pharm. Sci. Res., 2013, 4(3), 1227–1232.

  • Shashikant, A., Sunanda, A., Sachin, Z. and Padama, T., Quantification of intermediate unknown impurities and Z-isomer in entacapone API by HPLC. Int. J. Pharm. Sci. Res., 2015, 6(7), 3076–3082.

  • Naresh, K. and Madhuri, G. V., Stability indicating method of carbidopa and levodopa assay in carbidopa, levodopa and entacapone film coated tablets by RP-HPLC. Int. J. Pharm. Sci. Res., 2014, 5(12), 5530–5538.

  • Paim, C. S., Goncalvers, H. M. L., Miron, D. and Steppe, M., Stabilityindication LC determination of entacapone in tablets. J. Chromatogr., 2007, 65, 595–599.

  • Sekar, A., Ramaiyansekar and Nagaiah, K., Analytical methods for determination of entacapone in pharmaceuticals and urine. Eurasian J. Anal. Chem., 2015, 10(3), 150–162.

  • Bhatnagar, P., Vyas, D., Sinha, S. K. and Chakrabarti, T., Stability indicating HPLC method for simultaneous estimation of entacapone, levodopa and carbidopa in pharmaceutical formulation. J. Chromatogr. Sep. Techn., 2015, 6(7), 1–8.

  • Lakshmi, S., Lakshmi, K. S. and Rangarao, P., RP-HPLC estimation of entacapone in bulk and dosage form. J. Pharm. Res., 2009, 2(12), 1850–1851.

  • Maitreyi, Z., Bhavita, D. and Amit, K., Simultaneous estimation of levodopa, carbidopa and entacapone in pharmaceutical dosage by validated reverse phase high performance liquid chromatography. Int. J. Inst. Pharm. Life Sci., 2012, 2(1), 10–19.

  • Sravanthi, D., Anusha, M., Madhavi, S., Shaik, F. and Buchi, N. N., Simultaneous estimation of levodopa and carbidopa in bulk pharmaceutical dosage forms and dissolution sample analysis by RP-HPLC-PDA method. J. Chem. Pharm. Res., 2013, 5(11), 422–428.

  • Raja, A., Shyamsunder, M., David Bnji, C. H., Rao, K. N. V. and Selvakumar, D., Analytical method development and validation for simultaneous estimation of carbidopa, levodopa and entacapone in its bulk and tablet dosage form by UPLC. Int. Res. J. Pharm., 2013, 4(11), 53–56.

  • Ramakrishana, V., Balamuralikrishna, K. and Haribabu, B., Development and validation of liquid chromatographic method for the simultaneous estimation of levodopa, carbidopa and entacapone in the combined dosage form. J. Pharm. Res., 2014, 8(3), 281–288.

  • Praveen Kumar, T., Pallavi, Y., Deepthi, K. and Narayanaraju, P., Formulation and evaluation of entacapone sustained release matrix tablets. J. Pharma Innov., 2014, 3(8), 80–88.

  • Johan, B. and Kafil Dhingra, S., Stability indicating method for the determination of levodopa–carbidopa and related impurity. J. Chromatogr. A, 1994, 667(1–2), 175–181.

  • ICH validation of analytical procedures: text and methodology Q2 (R1), Current step 4 version, incorporated in November 2005; www.ich.org/fileadmin/Public_Web_Site/ICH.../Q2_R1/.../Q2_R1__Guideline.pdf

  • ICH impurities in new drug products Q3B (R2). Current step 4 version, dated 2 June 2006; www.ich.org/fileadmin/.../ICH_Products/.../Quality/Q3B_R2/.../Q3B_R2__Guideline


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  • Stability-Indicating Method of Entacapone-Related Substances Using UPLC in Finished Dosage Form

Abstract Views: 471  |  PDF Views: 117

Authors

Naresh Konduru
Department of Chemistry, GITAM University, Hyderabad 502 329, India
Rambabu Gundla
Department of Chemistry, GITAM University, Hyderabad 502 329, India
Naresh Kumar Katari
Department of Chemistry, GITAM University, Hyderabad 502 329, India
G. V. Madhuri
Department of Chemistry, GITAM University, Hyderabad 502 329, India

Abstract


A rapid, specific, sensitive and robust method for entacapone-related substances in carbidopa, entacapone and levodopa film-coated tablet was developed using ACQUITY UPLC with BEH C18 column. Mobile phase (A), i.e. 0.1% orthophosphoric acid and mobile phase (B), i.e. acetonitrile with water in the ratio 75 : 25 (v/v) with gradient method were employed. The method was evaluated for identification of process impurities and unknown impurities. It has been validated according to ICH (Q2) R1 guidelines. The values of LOD and LOQ for impurity and entacapone were found to be 0.01% and 0.03% respectively. Degradation studies were carried out in peroxide, acid, alkali conditions and contribution to mass balance was established. It was stable under heat, light-exposed and humid conditions.

Keywords


Entacapone-Related Substances, Dosage Form, Force Degradation Study, Liquid Chromatography.

References





DOI: https://doi.org/10.18520/cs%2Fv114%2Fi03%2F644-649