scholarly journals Green Stability Indicating Organic Solvent-Free HPLC Determination of Remdesivir in Substances and Pharmaceutical Dosage Forms

Separations ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 243
Author(s):  
Adel Ehab Ibrahim ◽  
Sami El Deeb ◽  
Emad Mahmoud Abdelhalim ◽  
Ahmed Al-Harrasi ◽  
Rania Adel Sayed
Keyword(s):  
Organic Solvent ◽  
Mobile Phase ◽  
Solvent Free ◽  
Chromatographic Technique ◽  
Lauryl Sulfate ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Liquid Chromatographic

A green liquid chromatographic method is considered in this work to minimize the environmental impact of waste solvents. One important principle is to replace or eliminate the use of hazardous organic solvents. Organic impurities in any active pharmaceutical ingredient could arise either during the process of its synthesis, or as degradation products developed throughout the shelf-life. Remdesivir (RDS) is an antiviral drug, approved by the US Food and Drug Adminstration (-FDA), to treat SARS-Cov-2 virus during its pandemic crisis. We studied the stability of remdesivir against several degradation pathways using the organic solvent-free liquid chromatographic technique. Separation was performed on RP-C18 stationary phase using mixed-micellar mobile phase composed of a mixture of 0.025 M Brij-35, 0.1 M sodium lauryl sulfate (SLS), and 0.02 M disodium hydrogen phosphate, adjusted to pH 6.0. The mobile phase flow rate was 1 mL min−1, and detection was carried out at a wavelength of 244 nm. We profiled the impurities that originated in mild to drastic degradation conditions. The method was then validated according to International Conference of Harmonization (ICH) guidelines within a linearity range of 5–100 μg mL−1 and applied successfully for the determination of the drug in its marketed dosage form. A brief comparison was established with reported chromatographic methods, including a greenness assessment on two new metrics (GAPI and AGREE). This study is the first to be reported as eco-friendly, solvent-free, and stability indicating LC methodology for RDS determination and impurity profiling.

scholarly journals Development and Validation of a Stability-Indicating Column High-Performance Liquid Chromatographic Assay Method for Determination of Nebivolol in Tablet Formulation

2008 ◽  
Vol 91 (3) ◽  
pp. 557-561 ◽  
Author(s):  
Pankaj K Kachhadia ◽  
Ashish S Doshi ◽  
Hitendra S Joshi
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Array Detector ◽  
Solution Stability ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A simple, precise, and accurate isocratic reversed-phase (RP) stability-indicating column high-performance liquid chromatographic (HPLC) assay method was developed and validated for determination of nebivolol in solid pharmaceutical dosage forms. Isocratic RP-HPLC separation was achieved on a Phenomenex Luna C8 (2) column (250 mm 4.6 mm id, 5 m particle size) using mobile phase composed of acetonitrilepH 3.5 phosphate buffer (35 + 65, v/v) at a flow rate of 1.0 mL/min, and detection was performed at 280 nm using a photodiode array detector. The drug was subjected to oxidation, hydrolysis, photolysis, and heat to apply stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The method was linear in the drug concentration range of 40160 g/mL with a correlation coefficient of 0.9999. The repeatability relative standard deviation (RSD) for 6 samples was 0.69, and the intermediate precision (RSD) for 6 samples was 1.39. The accuracy (recovery) was between 98.57 and 99.55. Degradation products produced as a result of stress studies did not interfere with detection of nebivolol, and the assay can thus be considered stability-indicating.

Analysis of Pharmaceutical Dosage Forms for Oxfendazole: II. Simultaneous Liquid Chromatographic Determination of Oxfendazole and Trichlorfon in Equine Paste

1986 ◽  
Vol 69 (1) ◽  
pp. 24-28
Author(s):  
Jeffrey Fleitman ◽  
Daniel Neu ◽  
Eric Benjamin
Keyword(s):  
Mobile Phase ◽  
Dimethyl Ester ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Organic Content ◽  
Phase Method ◽  
Pharmaceutical Dosage Forms ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract A reverse phase liquid chromatographic procedure is described for the simultaneous determination of oxfendazole [2-(methoxycarbonylamino)- 5-phenylsulfinylbenzimidazole] and trichlorfon [(2,2,2-trichloro-1-hydroxyethyl)phosphonic acid dimethyl ester] in equine paste. The sample is extracted by sonication in methanol. Insoluble excipients are removed by centrifugation and an aliquot plus internal standard are diluted with dilution solvent (water-acetonitrile-phosphoric acid, 80 + 20 + 1). The samples are filtered and injected onto a Partisil-5 ODS-3 column with acetonitrile-0.01M phosphate buffer pH 6.0 (20 + 80) as mobile phase. Method specificity is confirmed using an absorbance ratioing technique. The method yields mean recoveries of 100.9 and 100.0% for trichlorfon and oxfendazole, respectively. Dependence of chromatographic performance characteristics on mobile phase organic content, pH, and buffer concentration is also reported.

Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

2021 ◽  
Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Forms ◽  
Selective Determination ◽  
Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

Method Development and Validation of Degradation Studies of Lenalidomide by RP-HPLC

2021 ◽  
pp. 4281-4286
Author(s):  
Punna Venkateshwarlu ◽  
Mehul M. Patel
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
System Suitability ◽  
Wide Range

A simple, accurate, RP HPLC method was developed by this study determination of lenalidomide. This method is developed by Shimadzu LC -2010 HT by using C18 (250 X 4.6 X mm X 5µ) column in solvents Phosphate buffer: Acetonitrile (55:45) v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate 1ml/min was pumped and sample wavelength was detected at 242nm by ultraviolet -visible spectrophotometer. The retention time was found 2.5 min. The number of theoretical plates and tailing factor for lenalidomide was observed 16199.817 (NLT 2000) and 1.128 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, system suitability and robustness. LOD and LOQ values obtained from regression of lenalidomide 0.058 and 0.174µg/ml. The regression equation of validated method for lenalidomide is Y=5223x+183075. In wide range of 25 to 150 (µg/ml) the linearity was observed. The method was validated and a recovery study indicates accuracy of this method. The Retention time less compared to established methods. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lenalidomide in bulk drug and in its pharmaceutical dosage forms.

scholarly journals Simultaneous Determination of Acetaminophen, Pamabrom and Pyrilamine Maleate in Pharmaceutical Formulations Using Stability Indicating HPLC Assay Method

2017 ◽  
Vol 59 (2) ◽  
Author(s):  
Muhammad Ashfaq
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Water Ph

A simple, specific and accurate stability indicating RPHPLC method was developed for the determination of acetaminophen, pamabrom and pyrilamine maleate simultaneously in pharmaceutical dosage forms. Successful separation of all the components was enacted within 10 min using C18 column with mobile phase of methanol and acidified water (pH 1.8) in the ratio of (27: 73 v/v respectively). Flow rate of the mobile phase was 1.5 mL/min with detection at 300 nm. The method was validated in accordance with ICH guidelines. Response was a linear function of concentration over the range of 50- 150 􀈝g/mL for acetaminophen, 2.5-7.5 􀈝g/ mL for pamabrom and 1.5-4.5 􀈝g/mL for pyrilamine maleate. The method resulted in excellent separation of all the analytes along with their stress induced degradation products with acceptable peak tailing and good resolution. It is therefore can be applied successfully for simultaneous determination of acetaminophen, pamabrom and pyrilamine maleate in pharmaceutical formulations and their stability studies.

Stability-Indicating Methods for the Determination of Erdosteine in the Presence of its Acid Degradation Products

2014 ◽  
Vol 97 (1) ◽  
pp. 86-93 ◽  
Author(s):  
Nadia M Moustafa ◽  
Amr M Badawey ◽  
Nesrine T Lamie ◽  
Abd El-Aziz B Abd El-Aleem
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Validity Of Results ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Percentage Recovery ◽  
The Mean

Abstract Four accurate, sensitive, and reproducible stability-indicating methods for the determination of erdosteine in the presence of its acid degradation products are presented. The first method involves processing the spectra by using a first-derivative method at 229 nm in a concentration range of 10–70 μg/mL. The mean percentage recovery was 100.43 ± 0.977. The second method is based on ratio-spectra first derivative spectrophotometry at 227.4 and 255 nm over a concentration range of 10–70 μg/mL. The mean percentage recovery was 99.65 ± 1.122% and 100.02 ± 1.306% at 227.4 and 255 nm, respectively. The third method utilizes quantitative densitometric evaluation of the TLC of erdosteine in the presence of its acid degradation products, and uses methanol–chloroform–ammonia (7 + 3 + 0.01, v/v/v) asthe mobile phase. TLC chromatograms were scanned at235 nm. This method analyzes erdosteine in a concentration range of 2.4–5.6 μg/spot, with a mean percentage recovery of 100.03 ± 1.015%. The fourth method is HPLC for the simultaneousdetermination of erdosteine in the presence of its acid degradation products. The mobile phase consists of water–methanol (65 + 35, v/v). The standard curve of erdosteine showed good linearity overa concentration range of 10–80 μg/mL,with a mean percentage recovery of 99.90 ± 1.207%. These methods were successfully applied to the determination of erdosteine in bulk powder, laboratory-prepared mixtures containing different percentages of the degradation products, and pharmaceutical dosage forms. The validity of results was assessed by applying the standard addition technique. The results obtained agreed statistically with those obtained by a reported method, showing no significant differences with respect to accuracy and precision.

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