Optimization of RP-HPLC Assay for Pharmaceutical Analysis of Clopidogrel

DOI:

https://doi.org/10.37285/ijpsn.2014.7.1.9

Authors

  • Samer Housheh
  • Daoud Ali
  • Saleh Trefi
  • Haroun Mohammad
  • M. Fawaz Chehna

Abstract

An accurate, sensitive, precise and stability-indicating reversed phase high performance liquid chromatographic (RP-HPLC) method for the analysis of clopidogrel bisulfate was developed and validated. The chromatographic conditions comprised of a reversible phase C18 column (250 × 4.6 mm, 5 μm) with a mobile phase consisting of a mixture of 50 mM potassium di-hydrogen phosphate and acetonitrile in the ratio of 75:25 at pH 3.0 adjusted with phosphoric acid. The flow rate was 1ml/min, the detection was carried out at 247 nm and the retention time of clopidogrel was 6.5 min. Clopidogrel was subjected to acid and alkali hydrolysis, oxidation and photodegradation. The method was validated for accuracy, precision and robustness. The results indicate that the drugs are susceptible to degradation in different conditions. All the peaks of degraded products were resolved from the active pharmaceutical ingredient with significant different retention times. As the method could effectively separate the drug from its degradation products, it could be employed as a stability-indicating method.

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Keywords:

RP-HPLC, Clopidogrel, assay validation, degradation, stability indicating

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Published

2014-02-28

How to Cite

1.
Housheh S, Ali D, Trefi S, Mohammad H, Chehna MF. Optimization of RP-HPLC Assay for Pharmaceutical Analysis of Clopidogrel. Scopus Indexed [Internet]. 2014 Feb. 28 [cited 2024 Nov. 22];7(1):2371-6. Available from: https://ijpsnonline.com/index.php/ijpsn/article/view/702

Issue

Vol. 7 No. 1 (2014): January-March 2014

Section

Research Articles
Crossref
Scopus
Google Scholar
Europe PMC

References

Agrawal H, Kaul N, Paradkar AR and Mahadik KR (2003). Stability indicating HPTLC determination of Clopidogrel bisulphate as bulk drug and in pharmaceutical dosage form. Talanta 61: 581–589.

Antic D, Filipic S and Agbaba D (2007). A simple and sensitive TLC method for determination of Clopidogrel and its impurity SR 26334 in pharmaceutical product. ActaChromatogr 18: 199–206.

Bertand ME, Rupprecht HJ, Urban P and Gershlick AH (2000). Double-blind study of the safety of Clopidogrel with and without a loading dose in combination with aspirin compared with ticlopidine in combination with aspirin after coronary stenting: the Clopidogrel Aspirin Stent International Cooperative Study (CLASSICS). Circulation 102: 624–629.

CAPRIE Steering Committee (1996). A randomised, blinded, trial of Clopidogrel versus aspirin in patients at risk of ischaemic events. Lancet348: 1329–1339.

Chaudhari PB, Pawar PD and Narkhede KP (2010). Stability indicating spectrophotometric method for determination and validation of Clopidogrel bisulfate in tablet dosage form. Int J Res Ayur & Pharm 1(2): 418–423.

Dermis S and Aydogan E (2010). Electrochemical study of Clopidogrel and its determination using differential pulse voltammetry in bulk drug and pharmaceutical preparations. Pharmazie 65(3): 175–181.

Himani A, Neeraj K, Paradkar AR and Mahadik KR (2003). Stability indicating HPTLC determination of method for Clopidogrel bisulfate as bulk drug and in pharmaceutical dosage form. J Pharm & Biomed Anal 61: 581–589.

International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use. Note for guidance on stability testing: stability testing of new drug substances and products (CPMP/ICH/2736/99), ICH Topic Q1 A (R2) Stability Testing of new Drug Substances and Products.

International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use (1996). Validation of Analytical Procedures: Methodology. ICH-Q2B, Geneva, CPMP/ICH/281/95.

Jarvis B and Simpson K (2000). Clopidogrel: a review of its use in the prevention of atherothrombosis. Drugs 60:347–377.

Kample NS and Venkatachalan A (2005). Estimation of Clopidogrel from tablet dosage form by gas chromatography method. Indian J Pharm Sci 67: 128–129.

Mitakos A and Panderi I (2002). A validated LC method for the determination of clopidogrel in pharmaceutical preparations. J Pharm Biomed Anal 28(3-4): 431–438.

Pereillo JM, Maftouh M, Andrieu A, Uzabiaga MF, Fedeli O, Savi P, Pascal M, Herbert JM, Maffarand JP and Picard C (2002). Structure and stereochemistry of the active metabolite of clopidogrel. Drug Metab. Dispos 30:1288–1295.

Rajput SJ, George RK and Ruikar Deepthi B (2008). Chemometric simultaneous estimation of clopidogrel bisulfate and aspirin from combined dosage form. Indian J Pharm Sci 70: 450–454.

Rashmin BP, Madhira BS, Mrunali R and Kashyap PB (2008). Simultaneous estimation of acetylsalicylic acid and clopidogrel bisulfate in pure powder and tablet formulations by HPLC and HPTLC. J AOAC Int 91(4): 750–755.

Shah CR, Suhagia BN, Shah NJ, Patel DR and Patel NM (2008). Stability indicating simultaneous HPTLC method for olanzapine and fluoxetine in combined tablet dosage form. Indian J Pharm Sci 70(2): 251–255.

Yusuf S, Zhao F, Mehta SR, Chrolavicius S, Tognoni G and FoxKK (2001). Effects of clopidogrel in addition to aspirin in patients with acute coronary syndromes without ST-segment elevation. N Engl J Med 345:494–502.