Rapid and Accurate Determination of Clopidogrel in Tablets by Using Spectrophotometric and Chromatographic Techniques

Abstract

Quantitative determination of clopidogrel (CLP) was carried out by using zero-order and derivative ultraviolet (UV) spectroscopy. Calibration curves for CLP in 0.1N HCl between 0.1-0.8 mM (42-336 µg/mL) concentration range were obtained by the measurements at 267.5, 271.5 and 279.3 nm for first derivative, at 269.5, 273.4, 277.3 nm for second derivative and at 268.1, 271.3, 275.6 nm for third derivative UV spectrophotometry, respectively. In application, 270 nm in zero-order UV spectrophotometry, 279.3 nm in first derivative UV spectrophotometry, 269.5 nm in second derivative UV spectrophotometry and 275.6 nm in third derivative UV spectrophotometry were selected by their lowest relative standard deviation values in the validation studies. Mean recoveries and the relative standard deviations of the methods were found as 98.7 % and 1.90 % in zero-order UV spectrophotometry, 97.5 % and 0.76 % in first derivative UV spectrophotometry, 99.6 % and 1.25 % in second derivative UV spectrophotometry, 99.5 % and 1.15 % in third derivative UV spectrophotometry, respectively. In this study, the values of limit of detection and limit of quantitation were calculated at selected λ values as 0.01mM and 0.03 mM for zero-order (λ 270 nm), 0.02 mM and 0.07 mM for first derivative (λ 279.3 nm), second derivative (λ 269.5 nm), third derivative (λ 275.6 nm) UV spectrophotometry, respectively. The proposed methods were applied to the determination of CLP in bulk and tablets. The results were compared statistically with each other and high performance liquid chromatography (HPLC) procedure. The differences were not significant. In HPLC method, an isocratic system consisted of a Nova-Pak ® C18 analytical column and a mobile phase composed of pH 8 phosphate buffer : acetonitrile (30:70, v/v) at a flow rate 0.8 mL/min was used for the optimal chromatographic separation using UV detection at 210 nm. Applying HPLC method, linearity was observed in the concentration range from 1.26 to 7.55 µg/mL for CLP with a correlation coefficient 0.999. The values of the limit of detection and limit of quantitation were calculated as 0.29 µg/mL and 0.96 µg/mL, respectively. Synthetic samples were analyzed and mean recoveries and the relative standard deviations were found as 99.95 % and 0.40 % in HPLC. The spectrophotometric methods presented in this study can be used accurate, simple, economic and practical in the determination of CLP in tablets. The procedures do not require any separation step. The mean recoveries were found satisfactory in the methods. These methods also give repeatable results. Proposed methods could usefully be applied to routine quality control of tablets containing CLP. No interference was observed from common excipients in pharmaceutical formulations.

A Novel Strategy for Quantifying Clopidogrel Using Square‐wave Voltammetry and a Boron‐doped Diamond Film

“…The pH measurements were realized at 25.0 � 1.0 °C using a combined glass electrode with an Ag/AgCl In order to check the accuracy of proposed method, spectrophotometric determination of CLO was carried out using a ThermoSpectronic spectrophotometer UVvisible (model Genesys), employing a 1 cm quartz cell, as described by DERMIS, S. and AYDOGAN, E. [16].…”

“…There are few articles in the literature that describe the determination of CLO in pharmaceutical formulations, human urine and blood serum samples. DERMIS and AYDOGAN [16] developed a voltammetric method for the determination of CLO using a GCE, with acetate buffer (pH 3.7) as the electrolyte. Through the optimized DPV conditions they obtained a linearity between the CLO concentration and the peak current in the range from 80 to 1000 μmol L À 1 and a detection of limit (LOD) of 19.1 μmol L À 1 .…”

“…The most commonly used techniques in the determination of CLO are gas and liquid chromatography with detection by ultraviolet spectroscopy and mass spectrometry [10][11][12][13][14][15] and ultraviolet spectroscopy [16,17]. However, these techniques make excessive use of organic solvents, which generate an environmental impact, use expensive equipment and require long-time for the analysis, mainly due to the preparation of the sample, and they are therefore not feasible for routine analysis.…”

Comparative Study of Rp-HPLC Method Versus Fourier Transform Convolution Chemometric Methods; An Application on Pharmaceutical Binary Mixtures of Candesartan Cilexetil-Pitavastatin Calcium and Clopidogrel Bisulfate-Rosuvastatin Calcium

“…Literature revealed a variety of analytical methods for the determination of CLO alone or in combination with other drugs. CLO was determined alone by spectrophotometry [5], HPLC [6], LC-MS [7], LC-MS-MS [8]. CLO has also been assayed in combination with other drugs by spectrophotometry [9], chemometric methods [10,11], HPLC [12].…”

Determination of clopidogrel using square wave voltammetry at a gold electrode

“…5 2132 MLADENOVIĆ et al Analytical methods for the determination of clopidogrel include mostly chromatographic and spectrophotometric techniques: gas chromatography-mass spectrometry (GC-MS), 6 liquid chromatography-mass spectrometry (LC-MS), [7][8][9][10] high-performance liquid chromatography (HPLC), [11][12][13] liquid chromatography, 14 LC-MS/MS, 15 LC-ESI-MS/MS, 16 thin-layer chromatography (TLC), 17 high-performance thin-layer chromatography (HPTLC), 18 UV spectrophotometry. [19][20][21][22][23][24] Furthermore, the determination of clopidogrel and its impurities by capillary electrophoresis was reported. 25 Electrochemical determination of clopidogrel in standard form and pharmaceutical preparations using the differential pulse voltammetry (DPV) method with a glassy carbon working electrode was recently published.…”