scholarly journals Determination of Possible Potential Genotoxic Impurities in Lenalidomide Drug Substance by Simple RP-HPLC Method

2020 ◽  
Vol 32 (12) ◽  
pp. 2965-2970
Author(s):  
Kishore Gaddam ◽  
Shanker Kanne ◽  
Trivikram Reddy Gundala ◽  
Yogeshwar Reddy Mamilla ◽  
Gangi Reddy Nallagondu Chinna
Keyword(s):  
Simultaneous Detection ◽  
Acid Methyl Ester ◽  
Hplc Method ◽  
Uv Detector ◽  
Nitrobenzoic Acid ◽  
Rp Hplc ◽  
Genotoxic Impurities ◽  
Precision System ◽  
Development And Validation

This study is concerned with development and validation of HPLC method for the simultaneous detection and quantification of methyl 2-(chloromethyl)-3-nitrobenzoate (MCN), methyl 2-(bromomethyl)-5-nitrobenzoate (MMM), methyl 2-(bromomethyl)-6-nitrobenzoate (MON), methyl 2-(bromomethyl)-4-nitrobenzoate (MPN) and 2-methyl-3-nitrobenzoic acid methyl ester (MNM), which are the genotoxic impurities of lenalidomide. Chromatographic separation was accomplished using a Waters HPLC system equipped with Ascentis Express F5 (150 × 4.6 mm, 2.7 μm) using mobile phase composed of solvent A (0.1% perchloric acid): solvent B (methanol 80% and acetonitrile 20%); 55:45, vol/vol. The selected impurities were detected using UV detector set at 210 nm. The standard curves showed linearity in the range of concentrations 4.59-91.2 ppm (for MCN), 6.58-90.0 ppm (for MMM), 3.96-89.1 ppm (for MON), 6.47-89.7 ppm (for MPN) and 4.28-90.1 ppm (for MNM). The statistical results of method precision, system precision, specificity, accuracy, ruggedness was found to be within limits of acceptance. All the impurities were stable in lenalidomide test samples up to 24 h.

scholarly journals Development and validation of a new analytical RP-HPLC method for simultaneous determination of Glibenclamide and Atenolol in bulk

2019 ◽  
Vol 10 (3) ◽  
pp. 2433-2445
Author(s):  
Anitha P ◽  
Ramkanth S ◽  
Satyanarayana S V
Keyword(s):  
Hplc Method ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Development And Validation ◽  
First Time

A new, simple, reliable, fast, sensitive and economical RP-HPLC method was developed and validated for simultaneous estimation of two fixed-dose combinations frequently prescribed in coexisted chronic diseases such as diabetes (GLB) and hypertension (ATN) in bulk for the first time. The mobile phase used for the chromatographic runs consisted of 0.01N potassium dihydrogen ortho phosphate (pH 4.8) and acetonitrile (55:45, v/v). The separation was achieved on column (BDS C18 250 x 2.1mm, 1.6m) using isocratic mode. Drug peaks were well separated and were detected by a UV detector at 235.0 nm. The method was linear at the concentration range 2.5-15µg/ml for Glibenclamide (GLB) and 6.25-37.5µg/ml for Atenolol (ATN), respectively. The method has been validated according to ICH guidelines with respect to system suitability, specificity, precision, accuracy and robustness. The method was validated for system suitability, linearity, accuracy, precision, detection, quantification limits and robustness and was found it is acceptable in the range of 2.5–15 µg/ml for GLB and 6.25–37.5 µg/ml for ATN. The LOD and LOQ of GLB was found to be 0.48 µg/ml and 1.47µg/ml and for ATN was found to be 0.72µg/ml and 2.20 µg/ml, respectively. The method was applied to drug interaction studies of GLB with ATN to illustrate the scope and application of the methods to manage two different therapeutic classes of drugs, as they may co-administered in concurrent diseases.

scholarly journals Development and validation of a fast and simple RP-HPLC method for the determination of diosmin and hesperidin in combined tablet dosage form

2018 ◽  
Vol 37 (2) ◽  
Author(s):  
Marjan Piponski ◽  
Tanja Bakovska Stoimenova ◽  
Marina Topkoska ◽  
Stefan Stefov ◽  
Magdalena Piponska ◽  
...  
Keyword(s):  
Retention Time ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Time Cycle ◽  
Development And Validation ◽  
Tablet Dosage

A fast, simple, accurate and robust reversed phase HPLC method for the simultaneous determination of two flavonoids, hesperidin and diosmin, in combined tablets was developed and validated. This method uses a short C8 column with dimensions of 75 mm × 4 mm with 5 µm particles thermostated at 30 °C, and a mobile phase composed of formic acid (pH 4.1 and 0.05%, V/V) and methanol (58:42, V/V), delivered at a flow rate of 1.2 ml/min, with UV detector signal monitoring at 280 nm and an injection volume of 5 µl. These chromatographic conditions yielded chromatograms with symmetric peaks of hesperidin, eluting at a ~2 min retention time, and diosmin, at a ~4.5 min retention time, with a total run time cycle of 6 min. The method validation parameters confirmed excellent values for accuracy, linearity and reproducibility. This method is suitable for routine analysis in pharmaceutical and food quality control laboratories.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

A Development and Validation of RP-HPLC Method for the Determination of Degradation Impurities in Anagrelide Dosage Form

2021 ◽  
Vol 11 (5) ◽  
pp. 708-718
Author(s):  
Ravindra Mallavarapu ◽  
Kommera Pavithra ◽  
Naresh Kumar Katari ◽  
Thirupathi Dongala
Keyword(s):  
Dosage Form ◽  
Hplc Method ◽  
Rp Hplc ◽  
Development And Validation
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