Reverse Phase Liquid Chromatographic Method for the Quantification of Di-P-Toluoyl-D-Tartaric Acid in Escitalopram Oxalate Drug Substance
 
More details
Hide details
1
Post Graduate and Research Department of Chemistry, Islamiah College, Vaniyambadi, 635752, (Affiliated to Thiruvalluvar University, Vellore), India
2
Aurobindo Pharma Ltd Research centre, 313, Bachupally, Quthubullapur Mandal, Hyderabad-500 090, India
Publish date: 2017-11-01
 
Eurasian J Anal Chem 2011;6(3):197–205
KEYWORDS:
ABSTRACT:
A simple and rapid high performance liquid chromatographic method has been established to quantify the optically active precipitant Di-p-Toluoyl-d-Tartaric acid (DPTTA) at very low level in Escitalopram oxalate drug substance. The method is subsequently validated to prove its suitability, sensitivity and repeatability. The high performance liquid chromatographic (HPLC) method is developed in such a way that to enhances the detection level and minimizes acquisition time by using suitable buffer of 0.02% (v/v) of Orthophosphoric acid pH 3.0±0.5 and Acetonitrile as eluent in isocratic mode. The retention time of DPTTA is about 4.0 min and the total acquisition time was less than 15 min. The optimized method was validated to prove its performance characteristics by demonstrating selectivity, sensitivity (limit of detection and quantification), linearity, precision and accuracy. The experimentally established limit of detection and quantification was found to be 0.040 μg mL-1 and 0.120 μg mL-1 respectively and the overall percent accuracy (recovery) of the samples evaluated at different concentration levels was found to be 99.0, indicating the sensitivity and accuracy of this optimized HPLC method by citing the guideline requirement.
CORRESPONDING AUTHOR:
Tarkatti Kaleemullah   
Post Graduate and Research Department of Chemistry, Islamiah College, Vaniyambadi, 635752, (Affiliated to Thiruvalluvar University, Vellore), India
 
REFERENCES (18):
1. Hyttel J (1982) Citalopram-Pharmacological profile of a specific serotonin uptake inhibitor with antidepressant activity. Progress in Neuro-Psychopharmacology and Biological Psychiatry 6(3): 277-295.
2. Gravem A, Amthor K F, Astrup C, Elgen K, Gjessing L R, Gunby B, Pettersen R D, Kyrdalen L, Vaadal J, Ofsti E, Aarvold A (1987) A double-blind comparision of Citalopram (Lu 10- 171) and Amitriptyline in depressed patients. Acta Pshychiatrica Scandinavica 75(5): 478- 486.
3. Sanchez C, Bogeso K P, Elbert B, Reines E H, Braestrup C (2004) Escitalopram versus Citalopram: The surprising role of the R-enantiomer. Psychopharmacology (Berl.) 174 (2): 163-76.
4. Chen F, Larsen M B, Sanchez C, Wiborg O (2005) The S-enantiomer of R,Scitalopram, increases inhibitor binding to the human serotonin transporter by an allosteric mechanism, Comaprison with other serotonin transporter inhibitors. Eur Neuropsychopharmacol 15 (2): 193-8.
5. Margoob M A, Mushtaq D, Murtaza I, Mushtaq H, Ali A (2008) Serotonin transporter gene polymorphism and treatment response of serotonin reuptake inhibitör (escitalopram) in depression: Open pilot study. Indian J Psychiatry 50 (1): 47-50.
6. Owens M J, Knight D L, Nemeroff C B (2001) Second generation SSRI’s-human monoamine transporter binding profile of escitalopram and R-Fluoxetine. Biol Psychiatry 50 (5): 345-350.
7. Elati C R, Kolla N, Vankawala P J, Gangula S, Chalamala S, Sundaram V, Bhattacharya A, Vurimidi H, Mathad V T (2007) Substrate Modification Approach to Achieve Efficient resolution: Didesmethylcitalopram: A key intermediate of Escitalopram.Org Process Res Dev 11 (2): 289-292.
8. Dancer R J, de Diego H L (2009) Attempted Resolution of citalopram using (-)-O-O’-Di-p-toluoyl-(R,R)-tartaric acid and reflections on an alkylation reaction: Comment on an article by Elati et.al. Org Process Res Dev 13 (1): 23-33.
9. Mahadik M V, Dhaneshwar S R, Kulkarni M J (2007) Application of Stability Indicating HPTLC Method for Quantitative Determination of escitalopram Oxalate in Pharmaceutical Dosage Form. Eurasian J Anal Chem 2 (2): 101-117.
10. Sungthong B, Jac P, Scriba G K E (2008) Development and validation of a capillary electrophoresis method for the simultaneous determination of impurities of escitalopram including the R-enantiomer. J Pharm Biomed Anal 46 (5): 959-965.
11. Vetrichelvan T, Arul K, Sumithra M, Umadevi B (2010) Colorimetric method for the estimation of escitalopram oxalate in tablet dosage form. Indian J Pharm Sci. 72(2): 269-271.
12. Greiner C, Hiemke C, Bader W, Haen E (2007) Determination of citalopram and escitalopram together with their active main metabolites desmethyl(es-)citalopram in human serum by column-switching high performance liquid chromatography and spectrophotometric detection. J Chromatogr B Analyt Technol Biomed Life Sci 848 (2): 391-394.
13. Taha E A, Salama N N, Wang S (2009) Micelle Enhanced Fluorimetric and Thin Layer Chromatography Densitometric Methods for the Determination of (±) Citalopram and its S-Enantiomer escitalopram. Anal Chem Insights 4: 1-9.
14. Raman B, Sharma B A, Ghugare P D, Nandavadekar S, Singh D, Karmuse P K, Kumar A (2010) Structural elucidation of process-related impurities in escitalopram by LC/ESI-MS and NMR. J Pharm Biomed Anal 53(4): 895-901.
15. International conference on harmonization Q3A (R2): Draft revised Guidance on impurities in new drug substances; 2006.
16. Snyder L R, Krikland J J, Glajch J L (1997) Practical HPLC Method Development, 2nd Edition, John Wiley & Sons, New York, NY, 236-260.
17. ICH harmonized tripartite guideline. Validation of Analytical procedures Text and methodology Q2 (R1), 2005.
18. International Conference on Harmonization of Technical Requirement for Registration of Pharmaceuticals for Human use. ICH harmonized tripartite guideline, Stability testing of new drug substances and products Q1A (R2) 2003.
eISSN:1306-3057