Application of Quality by Design in the Development of HPTLC Method for Estimation of Anagliptin in Bulk and in-house Tablets
More details
Hide details
R. C. Patel Institute of Pharmaceutical Education and Research, INDIA
Amod Shivaji Patil   

Department of Pharmaceutical Chemistry, R.C. Patel Institute of Pharmaceutical Education and Research, Shirpur, Dist. Dhule, (MS), India 425 405, Near Karwnad Naka, 425405 Shirpur, India
Online publication date: 2017-01-05
Publication date: 2017-01-05
Eurasian J Anal Chem 2017;12(5):443–458
This paper comprehends systematic Quality by Design (QbD) based development of Normal-Phase High-Performance Thin-Layer Chromatography (NP-HPTLC) method for qualitative and quantitative estimation of anagliptin in bulk and in-house tablets. Chromatographic separation was executed out on aluminum backed Silica gel F254 plates using dichloromethane: methanol (9.2:0.8 v/v) as a mobile phase. Densitometry scanning was accomplished at 248 nm. Quality target method profile was defined and critical analytical attributes (CAAs) for the HPTLC method set aside. The mobile phase ratio and saturation time were determinate as critical method parameters (CMPs) and systematically optimized using Central composite design, evaluating for CAAs, namely retention factor (Rf), Peak-area and Peak-height. Statistical modelization was implemented followed by response surface analysis for comprehending plausible interaction(s) among CMPs. Search for optimum solution was conducted through numerical and graphical optimization for demarcating the design space. The described method was linear. The precision, ruggedness, and robustness values were also within the prescribed limit. The studies successfully demonstrate the utility of QbD approach for developing the highly sensitive HPTLC method with enhanced method performance.
Kato, N., Oka, M., Murase, T., Yoshida, M., Sakairi, M., Yamashita, S., Yasuda, Y., Yoshikawa, A., Hayashi, Y., Makino, M., Takeda, M., Mirensha, Y., & Kakigami, T. (2011). Discovery and pharmacological characterization of N-[2-({2-[(2S)-2-cyanopyrrolidin- 1-yl]-2-oxoethyl}amino)-2-methylpropyl]-2-methylpyrazolo[1,5-a]pyrimidine- 6-carboxamide hydrochloride (anagliptin hydrochloride salt) as a potent and selective DPP-IV inhibitor. Bioorganic & Medicinal Chemistry Letters, 19, 7221.
Kim, W., & Egan, J. M. (2008). The role of incretins in glucose homeostasis and diabetes treatment. Pharmacological Reviews, 60, 470.
Holst, J. J., Vilsboll, T., & Deacon, C. F. (2009). The incretin system and its role in type 2 diabetes mellitus. Molecular and cellular Endocrinology, 297, 127.
Mentlein, R., Gallwitz, B., & Schmidt, W. E. (1993). Dipeptidyl-peptidase IV hydrolyses gastric inhibitory polypeptide, glucagon-like peptide-1(7-36)amide, peptide histidine methionine and is responsible for their degradation in human serum. European Journal of Biochemistry, 214, 829.
International Conference on Harmonization of technical requirements for registration of pharmaceuticals for human use, ICH harmonized tripartite guideline, Pharmaceutical Development. (2008). Q8 (R1).
International Conference on Harmonization of technical requirements for registration of pharmaceuticals for human use, ICH harmonized tripartite guideline, Quality Risk Management. (2005). Q9.
International Conference on Harmonization of technical requirements for registration of pharmaceuticals for human use. ICH harmonized tripartite guideline, Pharmaceutical Quality Systems (2008). Q10.
Peraman, R., Bhadraya, K., & Reddy, Y. P. (2015). Analytical Quality by Design, A Tool for Regulatory Flexibility and Robust Analytics. International Journal of Analytical Chemistry 2015, 1.
Elder, P., & Borman, P. (2013). Improving analytical method reliability across the entire product lifecycle using QbD approach. Pharmaceutical Outsourcing, 14(4), 14.
Borman, P., Chatfield, M., Nethercote, P., Thompson, D., & Truman, K. (2007). The application of quality by design to analytical methods. Pharmaceutical Technology, 31(12), 142.
Vogt, F. G., & Kord, A. S. (2011). Development of quality-by-design analytical methods. Journal of Pharmaceutical Sciences, 100(3), 797.
Beg, S., Sharma, G., Katare, O. P., Lohan, S., & Singh, B. (2015). Development and Validation of a Stability-Indicating Liquid Chromatographic Method for Estimating Olmesartan Medoxomil using Quality by Design. Journal of Chromatographic Science, 73(7), 1048.
Bhoop, B. S. (2014). Quality by Design (QbD) for Holistic Pharma Excellence and Regulatory Compliance. Pharma Times, 46(08), 26.
Fahmy, R., Kona, K., Dandu, R., Xie, W., Claycamp, G., & Hoag, S. W. (2012). Quality by Design I, Application of Failure Mode Effect Analysis (FMEA) and Plackett–Burman Design of Experiments in the Identification of “Main Factors” in the Formulation and Process Design Space for Roller-Compacted Ciprofloxacin Hydrochloride Immediate-Release Tablets. AAPS Pharm SciTech, 13(4), 1243.
Majithia, R. H., Shah, J. S., & Maheswari, D. G. (2015). Development and Validation of Analytical Method for Estimation of Anagliptin in Tablet Dosage Form by UV Spectrophotometric Method. International Journal of Pharmaceutical Technology, 6(4), 7765.
Singh, B., Raza, K., & Beg, S. (2013). Developing optimized drug products employing designed experiments. Chemical Industry Digest, 6, 70–76.
Singh, B. (2005). Optimizing Drug Delivery Systems Using Systematic Design of Experiments Part I, Fundamental Aspects. Critical Reviews in Therapeutic Drug Carrier Systems, 22(1), 27.