A Validated Stability Indicating HPTLC Method for Determination of Aspirin and Clopidogrel Bisulphate in Combined Dosage Form
More details
Hide details
AISSMS College of Pharmacy, Kennedy Road, Maharashtra, India
Mrinalini C. Damle   

AISSMS College of Pharmacy, Kennedy Road, Maharashtra, India
Publish date: 2017-10-06
Eurasian J Anal Chem 2009;4(2):152–160
A sensitive, selective, precise and stability indicating (in accordance with ICH guidelines) High-Performance Thin Layer Chromatographic method of analysis for Aspirin and Clopidogrel bisulphate was developed, to resolve drugs response from that of their degradation products. The method employed TLC aluminum plates precoated with silica gel 60 F254 as the stationary phase. The solvent system consisted of carbon tetrachloride-acetone (6: 2.4 v/v). This system was found to give compact spots for both Aspirin and Clopidogrel bisulphate (Rf value 0.13±0.02, 0.78±0.02 respectively). Both the drugs were subjected to stress test conditions like acid/ alkali/ neutral hydrolysis, oxidation, dry heat treatment and photo degradation. The spots for product of degradation were well resolved from the spot of respective drugs. Densitometric analysis of drugs was carried out in the absorbance mode at 220 nm. The linear regression data for the calibration plots showed good linear relationship with r2 0.9991 and 0.9866 in the concentration range of 200-600 ng/spot and 300-600 ng/spot for Aspirin and Clopidogrel bisulphate, respectively. The results indicate that the drugs are susceptible to degradation, to different extent in different conditions.
Tripathi K D (2004) Essentials of Medical Pharmacology, 5th edition, Jaypee Brothers Medical publishers (P) ltd: New Delhi, p 560.
Satoskar R S, Bhandarkar S D, Ainepure S S (1997) Pharmacology and Pharmacotherapeutics, 3rd edition, Mumbai Prakashan: Mumbai, p 462.
O’ Neil M J, Smith Ann (2001) The Merck Index, 13th edition Merck and Co., INC. Whitehouse station: New Jersey, p 856 & 2421.
Tang M, Yang M M, Jian C N (2006) Antipalet agents Aspirin and Clopidogrel are Hydrolysed by Distinct Hydroxylesterases and Clopidogrel is Transesterificated in the presence of ethyl alcohol. Journal of Pharmacology and Experimental Therapeutics, 319: 1467-1476.
Ahmed B H U, Sadik G (2001) Development of a spectrometric method for the Determination of Aspirin in Blood sample. Journal of Medical Sciences 1: 61-62.
Satinsky D, Net I and Solich P (2004) Sequential inject chromatographic determination of paracetamol, caffeine and Acetyl salicylic acid in Pharmaceutical Tablets. Journal of Seperation Science, 27: 529-536.
Pandiyan K M, Shanmuga P, Anbazhagan S (2004) RP-HPLC method for simultaneous estimation of Atorvastatin and Aspirin from Capsule formulation. Indian Drugs, 41: 284-289.
Umapathi P, Parimoo P, Thomas S K (1997) Spectrometric estimation of Aspirin and Dipyridamole in pure admixture and in dosage forms. Journal of Pharmaceutical and Biomedical Analysis 15: 1703-1708.
Mishra P, Dolly A (2005) Development of UV Spectrophotometric method for the determination of Clopidogrel in tablet dosage form. Indian J Pharm Sci 67: 491-493.
Mitkos A, Panderi I A (2002) Validation LC method for the determination of Clopidogrel in pharmaceutical preparation. Journal of Pharmaceutical and Biomedical Analysis 28: 431-438.
Agrawal H, Kaul N, Paradkar (2005) A Stablity indicating HPTLC determination of Clopidogrel bisulphate as bulk drug and in pharmaceutical dosage form. Talanta 61: 581-589.
Kample N S, Venkatachalan A (2005) Estimation of Clopidogrel from tablet dosage form by gas chromatography method, Indian J Pharm Sci 67: 128-129.
Anandakumar K, Ayyappan T, Raman V R (2007) RP-HPLC analysis of Aspirin and Clopidogrel bisulphate in combination, Indian J Pharm Sci 69: 597-560.
Validation of Analytical Procedures: Text and Methodology Q1A (R2), ICH Harmonized Tripartite Guideline, Feb 2003.
Stability Testing of New Drug Substances and Products Q2 (R1), ICH Harmonized Tripartite Guideline, Nov 2005.