RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ASPIRIN AND PRASUGREL IN BINARY COMBINATION
Abstract
A simple, reliable, rapid, precise, sensitive and validated RP-HPLC method has been developed to determine Aspirin and Prasugrel in synthetic mixture form. Chromatographic separation achieved isocratically on Luna C18 column (5µm, 150mm × 4.60mm) and acetonitrile: 0.05M ammonium acetate buffer (pH 4.5) in the ratio of 75:25 (v/v) as the mobile phase, at a flow rate of 0.6 ml/min. Detection was carried out at 245 nm. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the ICH guidelines. The retention times for Aspirin and Prasugrel was found to be 2.25±0.5 and 8.72±0.5 min respectively. Linearity for Aspirin and Prasugrel was in the range of 75-375μg/ml and 10-50μg/ml respectively. The mean recoveries obtained for Aspirin and Prasugrel were 99.58 and 99.48 % respectively and RSD was less than 2. The correlation coefficients for all components are close to 1. Developed method was found to be accurate, precise, selective and rapid for simultaneous estimation of Aspirin and Prasugrel.
Keywords:
Aspirin, Prasugrel, RP-HPLC, ValidationDOI
https://doi.org/10.25004/IJPSDR.2012.040310References
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31. Jena FM, Ravi Kumar BVV, Viriyala RK, Annapurna MM, Bisht SPS. Validated new spectrophotometric methods for the estimation of prasugrel in bulk and pharmaceutical dosage forms. Int. J. Compr. Pharm. 2011; 6:1-3
32. Kumar AA, Kumar AA, Gowri Sankar D. Development, estimation and validation of prasugrel in bulk and in its pharmaceutical formulation by UV-vis spectroscopic method. Pharmanest. 2011; 2: 37-39.
33. Mohammed Ishaq B, Vanitha Prakash V, Krishna Mohan G. Development and validation of HPLC method for determination of Prasugrel in bulk and its pharmaceutical formulation. J. Chem. Pharm. Res. 2011; 3:404-409.
34. Prabahar AE, Rama Rao N, Sambasiva Rao KRS, Vijayaraj Kumar P. Method development and validation for the HPLC potency assay of prasugrel tablets. J. Pharm. Res. 2011; 4:980-982.
35. Wickremsinhe ER, Tian Ye, Ruterbories KJ, Verburg EM, Weerakkody GJ, Kurihara A, Farid NA. Stereoselective metabolism of prasugrel in humans using a novel chiral liquid chromatography-tandem mass spectrometry method. Drug. Metab. Dispos. 2007; 35: 917-921.
36. Farid NA, McIntosh M, Garofolo F, Wong E, Shwajch A, Kennedy M, Young M, Sarkar P, Kawabata K, Takahashi M, Pang H. Determination of the active and inactive metabolites of prasugrel in human plasma by liquid chromatography/tandem mass spectrometry. Rapid. Commun. Mass. Spectrom. 2007; 21:169-79.
37. Lukram O, Zarapkar M, Jha CK, Parmar S, Tomar KS, Hande A. Electrospray ionization LC-MS/MS validated method for the determination of the active metabolite (R-138727) of prasugrel in human plasma and its application to a bioequivalence study. Drug. Test. Anal. 2012; 4: 58-166.
38. Borole TC, Mehendre R, Damle MC, Bothara KG. Development and validation of stability indicating HPTLC method for determination of Prasugrel, J. Chem. Pharm. Res.2010; 2:907-913.
39. Code Q2A-Text on Validation of Analytical Procedure Step-3 Consensus Guideline, 1994, ICH Harmonised Tripartite Guideline.
40. Code Q2B- Validation of Analytical Procedure Methodology Step-4 Consensus Guideline, 1994, ICH Harmonised Tripartite Guideline.
2. Mays DC, Sharp DE, Beach CA, Kershaw RA, Bianchine JR, Gerber N. Improved method for the determination of aspirin and its metabolites in biological fluids by high-performance liquid chromatography: applications to human and animal studies. J. Chromatogr. B: Biom. Sci. Appl. 1998; 311:301-309.
3. The Indian Pharmacopoeia, 4th ed. Vol. I, the controller of publications, New Delhi. 1996, pp. 69.
4. British Pharmacopoeia, International edition, Vol. II, HMSO, London. 1993, 780.
5. United States Pharmacopoeia, National Formulary USP23, Asian Edition, Rockville, MD: United States Pharmacopoeial Convention, Inc. 1995, pp. 133, 135, 1776, 1982.
6. Kokot Z, Burda K. Simultaneous determination of salicylic acid and acetylsalicylic acid in aspirin delayed release tablets formulation by second-derivative UV spectrophotometry. J. Pharma. Bio. Anal. 1998; 18:871-875.
7. Murtaza G, Khan SA, Shabbir A, Mahmood A, Asad MHHB, Farzana K, Malik NS, Hussain I. Development of a UV-spectrophotometric method for the simultaneous determination of aspirin and paracetamol in tablets. Sci. Res. Ess. 2011; 6: 417-421.
8. Gandimati M, Ravi TK, Abraham A, Thomas R. Simultaneous determination of aspirin and isosorbide 5-mononitrate in formulation by RP-HPLC. J. Pharm. Biomed. Anal. 2003; 32:1145-1148.
9. Franeta JT, Agbaba D, Eric S, Pavkov S, Aleksic M, Vladimirov E. HPLC assay of acetylsalicylic acid, paracetamol, caffeine and Phenobarbitals in tablets. I L Farmaco. 2002; 57:709-713.
10. Montgomery ER, Taylor S, Segretario J, Engler E. Development and validation of RP-HPLC method for analysis of aspirin and warfarin in combination. J. Pharm. Biomed. Anal. 1996; 15:73-82.
11. Frieder K, Doris J, Horst G. Simultaneous determination of acetylsalicylic acid and salicylic acid in human plasma by HPLC. J. Chromatogr B. 1996; 677:172-177.
12. Ramos-martos N, Aguirre-Gomez F, Monlina- Diaz A, Capitan-Vallvey LF. Application of liquid chromatography to the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thymine in pharmaceutical preparation. J. AOAC. 2001; 3:676-83.
13. Kumara P, Shukla S, Ganurea AL, Subudhia BB. Development and validation of a novel isocratic RP-HPLC method for simultaneous determination of atenolol and aspirin in fixed dose combinations. Der Pharma Chemica. 2011; 3: 13-21.
14. Anandakumar K, Ayyappan T, Raghu Raman V, Vetrichelvan T, Sankar ASK, Nagavalli D. RP-HPLC analysis of aspirin and clopidogrel bisulphate in combination. Indian J. Pharm. Sci. 2007; 69: 597-599.
15. Satinsky D, Neto I, Solich P, Sklenakova H, Conceicao M, Montenegro BS, Araujo AN. Sequential injection chromatographic determination of paracetamol, caffeine and acetyl salicylic acid in pharmaceutical tablets. J. Sep. Sci. 2004; 7:529-536.
16. Abu-Qare AW, Abou-Donia MB. A validated HPLC method for the determination of pyridostigmine bromide, acetaminophen, acetylsalicylic acid and caffeine in rat plasma and urine. J. Pharm. Biomed. Anal. 2001; 26: 939-947.
17. Tebbett IR, Omile CT, Danesh B. Determination of paracetamol, salicylic acid and acetyl salicylic acid in serum by high-performance liquid chromatography. J. Chromatogr B. 1985; 329: 196-8.
18. Yamamotoa E, Takakuwa S, Kato T, Asakawa N. Sensitive determination of aspirin and its metabolites in plasma by LC–UV using on-line solid-phase extraction with methylcellulose-immobilized anion-exchange restricted access media. J. Chromatogr B. 2007; 846:132-138.
19. Pirola R, Bareggi SR, Benedittis GD. Determination of acetylsalicylic acid and salicylic acid in skin and plasma by high-performance liquid chromatography. J. Chromatogr B. 1998; 705: 309-315.
20. Panchal HJ, Suhagia BN, Patel NJ. Simultaneous HPTLC analysis of atorvastatin calcium, ramipril and aspirin in capsule dosage form. J. Planar Chromatogr. 2009; 22:265-271.
21. Sinha PK, Damle MC, Bothra KG. A validated stability indicating HPTLC method for the determination of aspirin and clopidrogrel bisulphate in combined dosage form. Eur. J. Anal. Chem. 2009; 4:152-160.
22. Umapathi P, Parimoo P, Thomas SK, Agarwal V. Spectrofluorometric estimation of aspirin and dipyridamole in pure admixtures and in dosage forms. J. Pharm. Biomed. Anal. 1997; 15: 1703-1708.
23. Ahmed M, Biswas HU, Sadik G. Development of a spectrometric method for the determination of aspirin in blood samples. J. Med. Sci. 2001; 2:61-62.
24. Tsikasa D, Tewesa KS, Gutzkia FM, Schwedhelma E, Greipel J, Frolich JC. Gas chromatographic-tandem mass spectrometric determination of acetylsalicylic acid in human plasma after oral administration of low-dose aspirin and guaimesal. J. Chromatogr B. 1998; 709: 79-88.
25. Chang WC, Midodzi WK, Westerhout CM, Boersma E, Cooper J, Barnathan ES. Are international differences in the outcomes of acute coronary syndromes apparent or real, a multilevel analysis. J. Epidemiol. Comm. Health. 2005; 59:427-433.
26. Gupta M, Chang WC, Van de Werf F, Granger CB, Midodzi W, Barbash G. International differences in in-hospital revascularization and outcomes following acute myocardial infarction: a multilevel analysis of patients in ASSENT-2. Eur. Heart. J. 2003; 24:1640-50.
27. Giugliano RP, Llevadot J, Wilcox RG, Gurfinkel EP, McCabe CH, Charlesworth A. Geographic variation in patient and hospital characteristics, management, and clinical outcomes in ST-elevation myocardial infarction treated with fibrinolysis. Results from InTIME-II. Eur. Heart. J. 2001; 22:1702-1715.
28. Bassand JP, Hamm CW, Ardissino D, Boersma E, Budaj A, Fernandez-Aviles F. Guidelines for the diagnosis and treatment of non-ST-segment elevation acute coronary syndromes. Eur. Heart. J. 2007; 28:1598-660.
29. Silber S, Albertsson P, Aviles FF, Camici PG, Colombo A, Hamm C. Guidelines for percutaneous coronary interventions. The task force for percutaneous coronary interventions of the european society of cardiology. Eur. Heart. J. 2005; 26:804-847.
30. Wiviott SD, Braunwald E, McCabe CH, Montalescot G, Ruzyllo W ,Gottlieb S. Prasugrel versus clopidogrel in patients with acute coronary syndromes. N. Engl. J. Med. 2007; 357: 2001-2015.
31. Jena FM, Ravi Kumar BVV, Viriyala RK, Annapurna MM, Bisht SPS. Validated new spectrophotometric methods for the estimation of prasugrel in bulk and pharmaceutical dosage forms. Int. J. Compr. Pharm. 2011; 6:1-3
32. Kumar AA, Kumar AA, Gowri Sankar D. Development, estimation and validation of prasugrel in bulk and in its pharmaceutical formulation by UV-vis spectroscopic method. Pharmanest. 2011; 2: 37-39.
33. Mohammed Ishaq B, Vanitha Prakash V, Krishna Mohan G. Development and validation of HPLC method for determination of Prasugrel in bulk and its pharmaceutical formulation. J. Chem. Pharm. Res. 2011; 3:404-409.
34. Prabahar AE, Rama Rao N, Sambasiva Rao KRS, Vijayaraj Kumar P. Method development and validation for the HPLC potency assay of prasugrel tablets. J. Pharm. Res. 2011; 4:980-982.
35. Wickremsinhe ER, Tian Ye, Ruterbories KJ, Verburg EM, Weerakkody GJ, Kurihara A, Farid NA. Stereoselective metabolism of prasugrel in humans using a novel chiral liquid chromatography-tandem mass spectrometry method. Drug. Metab. Dispos. 2007; 35: 917-921.
36. Farid NA, McIntosh M, Garofolo F, Wong E, Shwajch A, Kennedy M, Young M, Sarkar P, Kawabata K, Takahashi M, Pang H. Determination of the active and inactive metabolites of prasugrel in human plasma by liquid chromatography/tandem mass spectrometry. Rapid. Commun. Mass. Spectrom. 2007; 21:169-79.
37. Lukram O, Zarapkar M, Jha CK, Parmar S, Tomar KS, Hande A. Electrospray ionization LC-MS/MS validated method for the determination of the active metabolite (R-138727) of prasugrel in human plasma and its application to a bioequivalence study. Drug. Test. Anal. 2012; 4: 58-166.
38. Borole TC, Mehendre R, Damle MC, Bothara KG. Development and validation of stability indicating HPTLC method for determination of Prasugrel, J. Chem. Pharm. Res.2010; 2:907-913.
39. Code Q2A-Text on Validation of Analytical Procedure Step-3 Consensus Guideline, 1994, ICH Harmonised Tripartite Guideline.
40. Code Q2B- Validation of Analytical Procedure Methodology Step-4 Consensus Guideline, 1994, ICH Harmonised Tripartite Guideline.
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01-07-2012
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“RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ASPIRIN AND PRASUGREL IN BINARY COMBINATION”. International Journal of Pharmaceutical Sciences and Drug Research, vol. 4, no. 3, July 2012, pp. 218-21, https://doi.org/10.25004/IJPSDR.2012.040310.
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How to Cite
“RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ASPIRIN AND PRASUGREL IN BINARY COMBINATION”. International Journal of Pharmaceutical Sciences and Drug Research, vol. 4, no. 3, July 2012, pp. 218-21, https://doi.org/10.25004/IJPSDR.2012.040310.
