AJAC  Vol.10 No.2 , February 2019
Determination and Validation of HPTLC Method for Cinacalcet Hydrochloride
ABSTRACT
Cinacalcet Hydrochloride (CIN) is a new calcimimetic agent indicated for the use in hypercalcemia. The present work is aimed at development and validation of a novel and simple high-performance thin-layer chromatographic (HPTLC) method for the analysis of Cinacalcet Hydrochloride (active pharmaceutical ingredient, API. In the method, Aluminum-backed silica gel 60 F254 plates (10 × 10 cm) were used as stationary phase and chloroform: acetonitrile (6:4, v/v) as the mobile phase, which showed compact bands of Cinacalcet HCl (RF 0.30 ± 0.02). Quantitative analysis was carried out by densitometry at a wavelength of 282 nm. Linear regression analysis for the calibration spots showed good correlation ship with regression co-efficient r2 = 0.9994 in the range of 40 - 160 ng/band. The developed method suitability for quantification of CIN was learned by validating it as per the ICH guidelines. CIN detection limit was 0.48 ng/band and the quantification limit was 1.59 ng/band. The proposed method was found to be linear (r2 = 0.999), precise (%RSD < 2% for intraday and intermediate precision), accurate, specific, and robust. Further, the developed method was validated and found suitable for stress induced studies, since presence of degradants has no effect on CIN estimation. The proposed method was found to be simple, sensitive, precise, accurate and reproducible for the estimation of CIN.
Cite this paper
Kamatham, S. and Veeresham, C. (2019) Determination and Validation of HPTLC Method for Cinacalcet Hydrochloride. American Journal of Analytical Chemistry, 10, 55-64. doi: 10.4236/ajac.2019.102005.
References
[1]   Franceschini, N., Joy, M.S. and Kshirsagar, A. (2003) Cinacalcet HCl: A Calcimimetic Agent for the Management of Primary and Secondary Hyperparathyroidism. Expert Opinion on Investigational Drugs, 12, 1413-1421.
https://doi.org/10.1517/13543784.12.8.1413

[2]   Torres, P.U. (2006) Cinacalcet HCl: A Novel Treatment for Secondary Hyperparathyroidism Caused by Chronic Kidney Disease. Journal of Renal Nutrition, 16, 253-258.
https://doi.org/10.1053/j.jrn.2006.04.010

[3]   Amgen Inc. (2015) Sensipar® (Cinacalcet) Tablets, Full prescribing Information.
http://pi.amgen.com/united_states/sensipar/sensipar_pi_hcp_english.pdf

[4]   Ravinder, V., Ashok, S., Varma, M.S., Babu, C.V.R., Shanker, K. and Balaswamy, G. (2009) A Validated Chiral LC Method for the Enantiomeric Separation of Cinacalcet Hydrochloride. Chromatographia, 70, 229-232.
https://doi.org/10.1365/s10337-009-1129-5

[5]   Ashok, S., Raghunath, C.H.V., Satish, M. and Balaswamy, G. (2009) Validated Liquid Chromatographic Method for the Determination of Impurities in Cinacalcet Hydrochloride. Analytical Chemistry (India), 8, 594-599.

[6]   Yang, F., Wang, H., Zhao, Q., Liu, H., Hu, P. and Jiang, J. (2012) Determination of Cinacalcet Hydrochloride in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry. Journal of Pharmaceutical and Biomedical Analysis, 61, 237-241.
https://doi.org/10.1016/j.jpba.2011.10.022

[7]   Darwish, I.A., AL-Shehri, M.M. and AL-Gendy, M.A. (2013) A Highly Sensitive HPLC Method with Non-Extractive Sample Preparation and Uv Detection for Trace Determination of Cinacalcet in Human Plasma. Digest Journal of Nanomaterials and Biostructures, 8, 1563-1570.

[8]   Radhika, T. and Prakash, K.V. (2013) Validated RP-HPLC Method for the Estimation of Cinacalcet in Bulk and Tablet Dosage Form. American Journal of PharmaTech Research, 3, 409-414.

[9]   Loni, A.B., Ghante, M.R. and Sawant, S.D. (2012) Spectrophotometric Estimation of Cincalcet Hydrochloride in Bulk and Tablet Dosage Form. International Journal of Pharmacy and Pharmaceutical Sciences, 4, 513-515.

[10]   Cangemi, G., Barco, S., Verrina, E.E., Scurati, S., Melioli, G. and Della Casa Alberighi, O. (2013) Micromethod for Quantification of Cinacalcet in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry Using a Stable Isotope-Labeled Internal Standard. Therapeutic Drug Monitoring, 35, 112-117.
https://doi.org/10.1097/FTD.0b013e318278dc69

[11]   Nirogi, R., Kandikere, V., Komarneni, P., Aleti, R., Padala, N. and Kalaikadiban, I. (2011) Quantification of Cinacalcet by LC-MS/MS Using Liquid-Liquid Extraction from 50 μL of Plasma. Journal of Pharmaceutical and Biomedical Analysis, 56, 373-378.
https://doi.org/10.1016/j.jpba.2011.05.032

[12]   Musharraf, S.G., Shoaib, M., Kumar, D. and Najam-ul-Haq, M. (2013) Effective Separation and Simultaneous Quantification of Permethrin Isomers in Household Products by Validated TLC-Densitometric Method. Journal of Planar Chromatography, 26, 14-20.
https://doi.org/10.1556/JPC.26.2013.1.2

[13]   Shardul, K., Kailas, C., Neha, S., Prafullachandra, T. and Ratnakar, L. (2014) A Validated High-Performance Thin Layer Chromatographic Method for the Determination of Azathioprine from Pharmaceutical Formulation. Journal of Planar Chromatography, 27, 120-123.

[14]   Mohammad, T., Zeenat, I., Javed, A., Sanjula, B., Rabea, P., Mohd Aamir, M., Sayeed, A. and Jasjeet Kaur, S. (2014) Development and Validation of Stability—Indicating High-Performance Thin Layer Chromatographic Method for the Simultaneous Quantification of Sparfloxacin and Flurbiprofen in Nanoparticulate Formulation. Journal of Planar Chromatography, 27, 124-131.

[15]   (2005) ICH Harmonised Tripartite Guideline: Validation of Analytical Procedures: Text and Methodology, Q2 (R1), Geneva.
http://www.ich.org/fileadmin/Pubic-web-site/ICH_products/guidelines/Quality/Q2-R1/step4/Q2-R1-Guideline.pdf

 
 
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