scholarly journals New High-Performance Liquid Chromatographic Method for Determination of Clopidogrel in Coated Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 67-72 ◽  
Author(s):  
Juliana Sippel ◽  
Letcia L Sfair ◽  
Elfrides E S Schapoval ◽  
Martin Steppe

Abstract A new high-performance liquid chromatographic method was developed and validated for clopidogrel determination in pharmaceutical formulations. The system consisted of an ACE 5 octadecylsilane (C18; 150 4.6 mm id), 5.0 m particle size column; methanol0.1 triethylamine (75 + 25, v/v), pH 5.3, mobile phase at a flow rate of 1.2 mL/min; and a diode array detector set at 220 nm. Specificity, linearity, precision, accuracy, and robustness were the parameters evaluated. The retention time for clopidogrel was 6.8 min. To estimate specificity, an aqueous sample solution was subjected to degradation by ultraviolet light and by acid, alkaline, and oxidation media. The peaks of degradation products did not interfere with the compound signal, and there was no interference when a placebo solution was analyzed. Linearity over a concentration range of 10.0 to 90.0 g/mL was shown (correlation coefficient = 0.9998). Low values of relative standard deviation indicated the adequate intraday and interday precision. The average recovery was found as 99.16. In the robustness test, small modifications to the mobile phase composition did not affect the determination of clopidogrel. The proposed method proved to be simple, fast, and cost efficient for the intended use.

2009 ◽  
Vol 92 (2) ◽  
pp. 404-409 ◽  
Author(s):  
Abdalla A Elshanawane ◽  
Samia M Mostafa ◽  
Mohamed S Elgawish

Abstract A high-performance liquid chromatographic method was developed for the simultaneous determination of 2 ternary mixtures containing amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone used in hypertension therapy. The use of cyanopropyl column results in satisfactory separation of both mixtures. The mobile phase consisted of 10 mM KH2PO4 buffer (pH 4.5) and methanol in a ratio of (75 25 v/v), at a flow rate of 1 mL/min. UV detector was operated at 275 nm. Calibration graphs were linear in the concentration ranges of 210, 20200, 10100, and 550 g/mL for amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone, respectively. Intraday and interday precision values (relative standard deviation) were <1.13 for mixture I (amiloride hydrochloride, atenolol, chlorthalidone), and <0.93 for mixture II (amiloride hydrochloride, atenolol, hydrochlorothiazide). The method was successfully applied for the determination of the 2 combinations in laboratory-prepared mixtures and commercial pharmaceutical formulation with high accuracy and precision. Statistical comparison of the results with those of the published methods showed excellent agreement and indicates no significant difference between them.


2019 ◽  
Vol 58 (2) ◽  
pp. 144-150
Author(s):  
Demet Dincel ◽  
Olcay Sagirli ◽  
Gulacti Topcu

Abstract In this study, a new, sensitive and selective high-performance liquid chromatographic method was developed for the determination of meropenem (MEM) in human serum. In the developed method, C18 column (3.9 × 150 mm, 5 μm) was selected as stationary phase at 30°C, and methanol: acetic acid solution mixture was used as mobile phase with gradient program. Chromatographic separation was carried out at a flow rate of 1 mL/min, and detection was performed at 300 nm with diode array detector. Doripenem was selected as an internal standard, and the analytes were extracted from serum using protein precipitation method with ortho-phosphoric acid: methanol. Detection wavelength was selected as 300 nm. The developed method was validated according to International Council for Harmonisation (ICH) guidelines. The calibration curve was linear over a concentration range of 4–240 μg/mL with correlation coefficient of 0.9985. The limit of detection and limit of quantification values were found as 0.057 and 0.192 μg/mL, respectively. The validated method was successfully applied for the determination of MEM in human serum samples collected from patient volunteers at different time intervals, and therapeutic drug monitoring of MEM has been investigated.


INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 67-71
Author(s):  
N Dhanvijay ◽  
◽  
Vijaya Kumar Munipalli ◽  
M. Patel ◽  
S. Ghani ◽  
...  

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic method has been developed for quantitative determination of antineoplastic drug bexarotene and its capsule formulation. In this method Synchronis (C18, 25cm×4.6mm id , 5μ) column with mobile phase consisting of buffer (25mM ammonium acetate w/v solution adjusted to pH 4.0 with diluted acetic acid) and acetonitrile in the ratio of (20: 80 v/v) in an isocratic mode was used. The detection was carried out at 262 nm and 20.0 μL injection volume was selected, with the flow rate of 1.0 mL/min being used. The linearity range of bexarotene shows concentration between 5-200 μg/mL. Retention time of bexarotene was found to be 12.58 minutes. Mobile phase itself was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of bexarotene in its formulation.


1984 ◽  
Vol 30 (6) ◽  
pp. 908-910 ◽  
Author(s):  
T Annesley ◽  
K Wilkerson ◽  
K Matz ◽  
D Giacherio

Abstract We describe a "high-performance" liquid-chromatographic method for simultaneously measuring various penicillin and cephalosporin antibiotics. After extraction from serum, which in general is quantitative, the drugs are separated by use of a "Bondapak phenyl" column and a gradient mobile phase. For these drugs retention times depend on the pH of the mobile phase; we present retention times under selected pH conditions.


Author(s):  
CAROLINE GRACE A ◽  
PRABHA T ◽  
SIVAKUMAR T

Objective: The aim of the present work is the development of new, sensitive, specific, and accurate high-performance liquid chromatographic method for the separation and determination of dapagliflozin and its impurities in tablet dosage form. Methods: The chromatographic separation of drug and its impurities was achieved using Hypersil BDS C18 column (250 mm × 4.6 mm, 5 μ) with mobile phase consisted of mobile phase-A (Buffer pH 6.5) and mobile phase-B (acetonitrile:water 90:10) by gradient program at a flow rate of 1 mL/min with ultraviolet detection at 245 nm. Results: Dapagliflozin and its impurities A, B, C, D, E, and impurity-F were successfully eluted at the retention time of 16.95, 2.72, 7.82, 10.58, 21.11, 30.37, and 34.36 min, respectively, with good resolution. The method was validated according to the international conference on harmonization guidelines. The validation results showed good precision, accuracy, linearity, specificity, sensitivity, and robustness. Conclusion: Successful separation and determination of dapagliflozin and its six impurities were achieved by the proposed method. The developed method can be applied for the routine analysis of dapagliflozin and its impurities in pharmaceutical formulations.


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