Validation of assay for bulk clopidogrel and for some tablet forms by reverse-phase high-performance liquid chromatography

Sahoo, Nalini Kanta; Sahu, Madhusmita; Rao, P. Srinivas; Indira, Jajula N.; Rani, Sandhya; Ghosh, Goutam

doi:10.1016/j.jtusci.2014.02.001

Cited by 7 publications

(5 citation statements)

References 8 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Regarding CLOP, an ofcial monograph was published for it in the USP and revealed that CLOP could be analyzed using a special column for HPLC analysis, and the absorbance is measured at 220 nm [16]. In addition, many studies have aimed to develop diferent methods of analysis of CLOP individually [17,18] or in combination using diferent technologies such as HPLC [19][20][21], ultra-high performance liquid chromatography (UHPLC) [22], UV spectrophotometric method [23], and thin layer chromatography (TLC) [24]. When performing our research, none of these studies had developed an analytical method for simultaneously determining APX and CLOP in the same dosage form using any spectrophotometric method.…”

Section: Introductionmentioning

confidence: 99%

HPLC Method Development and Validation for the Determination of Apixaban and Clopidogrel in Novel Fixed-Dose Combination Tablets

Al-Shami,

Naseef,

Moqadi

et al. 2024

Journal of Chemistry

View full text Add to dashboard Cite

A simple, fast, and accurate high-performance liquid chromatographic (HPLC) method is developed, optimized, and validated for a fixed-dose combination of apixaban (APX) and clopidogrel (CLOP) tablets according to ICH guidelines. Chromatographic separation of the drugs was performed on a BDS Hypersil C18 (4.6 ∗ 150 mm, 5 μm), with acetonitrile (ACN) and trifluoroacetic acid (TFA) in the ratio 48 : 52 (v/v) as a mobile phase, at a flow rate of 0.9 ml/min., injection volume of 5 μL, and column temperature 45°C. The proposed method was linear over the level 25–200% for a concentration of APX 5 μg/ml and CLOP 75 μg/ml (R2 > 0.999). The detection limit for APX and CLOP was found to be 0.3465 and 3.8496 μg/ml, whereas the quantification limit was 1.0499 and 11.6656 μg/ml, respectively. The recovery was more than 99% using the standard addition method. The developed method was found to be specific, accurate, precise, and robust against changes in column temperature (±5°C) and mobile phase composition (±5% ACN); hence, it can be used for the determination of APX and CLOP in the fixed-dose combination tablets.

show abstract

Section: Introductionmentioning

confidence: 99%

HPLC Method Development and Validation for the Determination of Apixaban and Clopidogrel in Novel Fixed-Dose Combination Tablets

Al-Shami,

Naseef,

Moqadi

et al. 2024

Journal of Chemistry

View full text Add to dashboard Cite

show abstract

“…The other degradation products are studied by reversed-phase HPLC [17] characterized by solid state stress conditions [18] and the structures are elucidated using LC-MS/TOF and LC-MS. Bulk clopidogrel and the tablet form are assayed by RP-HPLC [19], chemometry [20], spectrophotometry [21], TLC [22], HPTLC [23], normal phase LC [24] and squre wave voltammetry [25]. The redox behaviour was studied using cyclic voltammetry and differential pulse voltammetry techniques [26].…”

Section: Introductionmentioning

confidence: 99%

Electrochemical and Spectroscopic Studies of Interaction of Clopidogrel Bisulphate with Calf Thymus DNA

Malini¹,

Raj²,

Sennappan³

2017

Asian J. Chem.

View full text Add to dashboard Cite

The DNA binding properties of clopidogrel bisulphate, was examined by cyclic voltammetry, fluorescence and UV spectroscopy. Shift in peak potential, decrease in peak current in cyclic voltammetry, hypochromic effect in UV titration and quenched emission intensity of ethidium bromide bound to calf thymus DNA signal indicated clopidogrel bisulphate has displaced ethidium bromide from its binding site in DNA. The binding constant is calculated using absorbance and is found to be closer to that estimated in voltammetric measurements. The results also corroborated well with fluorescence measurements and represent that the binding proceeds by intercalation

show abstract

“…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].…”

Section: Introductionmentioning

confidence: 99%

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

Jamal

Gazy

2016

Int J Pharm Pharm Sci

View full text Add to dashboard Cite

Objective: A comparative study of smart spectrophotometric chemometric assisted techniques and RP-HPLC for the determination of candesartan cilexetil (CAN)-pitavastatin calcium (PIT) and clopidogrel bisulfate (CLO)-rosuvastatin calcium (ROS), binary co-administered drugs were developed and validated. Methods:The spectrophotometric chemometric assisted methods included two simple techniques, namely Fourier transform convolution (FF) and ratio spectra of Fourier transform convolution (FFR) methods. FFR is considered as a hybrid divisor ratio spectra method where Fourier functions are applied to divisor ratio signals. The RP-HPLC method involves a rapid separation on a C18 column using a mobile phase consisting of acetonitrile: sodium dihydrogen phosphate (adjusted to pH 2.6 using orthophosphoric acid) in the ratio of 70:30 v/v at a flow rate of 1 ml/min in isocratic mode. CLO and ROS were monitored at 220 nm however CAN and PIT were monitored at 238 nm. Results:The spectrophotometric chemometric assisted methods proved their ability to quantify each of the studied drugs in their binary mixtures, where excellent percentage recoveries were obtained. FF and FFR method proved to be linear over the concentration range of 10-50 µg/ml for CLO, 4-20 µg/ml for ROS, 8-20 µg/ml for CAN and 2-10 µg/ml for PIT. The RP-HPLC method was able to separate the drugs in the study; retention times were found to be 3.9 min and 14.4 min for ROS-CLO, 4.2 min and 14.5 min for PIT-CAN respectively. The RP-HPLC method was found to be linear in the concentration range of 0.1-0.5 µg/ml for CLO, 0.04-0.2 µg/ml for ROS, 0.5-1 µg/ml for CAN and 0.05-0.1 µg/ml for PIT. System suitability parameters proved that peaks were well resolved from each other. Conclusion:The spectrophotometric and chromatographic methods were validated according to ICH guidelines. Recovery was found to be in the range of 95.9 %-100.5 % in synthetic laboratory mixtures. The suggested spectrophotometric methods have the advantage over other methods that they do not require a preliminary separation. Statistical analysis between the suggested spectrophotometric chemometric assisted and RP-HPLC methods, using student's t-and F-test revealed that there is no difference between the applied methods.

show abstract

Validation of assay for bulk clopidogrel and for some tablet forms by reverse-phase high-performance liquid chromatography

Cited by 7 publications

References 8 publications

HPLC Method Development and Validation for the Determination of Apixaban and Clopidogrel in Novel Fixed-Dose Combination Tablets

HPLC Method Development and Validation for the Determination of Apixaban and Clopidogrel in Novel Fixed-Dose Combination Tablets

Electrochemical and Spectroscopic Studies of Interaction of Clopidogrel Bisulphate with Calf Thymus DNA

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

Contact Info

Product

Resources

About