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A Validated Enantioselective HPLC Method for Assay of S-Amlodipine Using Crown Ether as a Chiral Stationary Phase

[ Vol. 13 , Issue. 2 ]

Author(s):

Ahmed M. Abdel-Megied, Samia M. El-Gizawy, Osama H. Abdelmageed, Mahmoud A. Omar, Sayed M. Derayea and Hassan Y. Aboul-Enein   Pages 117 - 123 ( 7 )

Abstract:


Background: Hypertension represents a widespread cardiovascular condition although usually asymptomatic, is a major risk factor for myocardial ischemia, renal failure and stroke. Amlodipine is considered a powerful dihydropyridine calcium channel blocker used as antihypertensive agent. Its mechanism of action depend on relaxing the smooth muscle of the artery wall and decrease peripheral resistance.

Methods: An accurate, sensitive and robust chiral HPLC method was developed for separation and quantitation of S(-)- amlodipine simultaneously in the presence of its R(+)- isomer. Chiral separation was applied using Daicel CROWNPAK CR(+) (5µm, 4.0×150 mm) column which contains (3,3'-diphenyl-1,1'- binaphthyl)-20-crown-6-ether coated into a 5μm reversed phase silica support. The mobile phase system was aqueous acidic 70% HClO4 (pH 2.0) and methanol in the proportion of (95:5 v/v), filtered through 0.45 µm membrane and degassed by before use, pumped at a flow rate was 0.8 mL min-1 with UV detector adjusted at 238 nm.

Results: The chromatographic HPLC method was validated with respect to ICH guidelines. Linear concentration range was 5-60 µg mL-1 with correlation coefficient (r) about 0.9998, the detection and quantitation limits was found 1.66 and 5.05 µg m-1; respectively. Accuracy was evaluated using standard addition technique with mean recovery about 98.40 % while precision was assessed at intraday and interday level. It was found that all %RSD values below 2%.

Conclusion: A simple, enantioselective, chiral HPLC method was developed and validated for the quantitation of amlodipine [S-(+)- isomer] in racemic tablets using CROWNPAK CR(+) chiral stationary phase. The proposed method is specific, precise, accurate, and robust which can be successfully applied for the routine analysis of S-AML in bulk and pharmaceutical dosage formulations.

Keywords:

Amlodipine, Chiral analysis, HPLC, Crown ether, pharmaceutical analysis.

Affiliation:

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, October 6 University, 6th October City, Cairo, Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Assiut University, Assiut, Pharmaceutical Chemistry & Phytochemistry. Department, Faculty of Pharmacy, King Abdulaziz University, Jeddah, Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Pharmaceutical and Medicinal Chemistry Department, Pharmaceutical and Drug Industires Research Division, National Research Center, Dokki, Giza 12622

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