scholarly journals High Performance Liquid Chromatography Method for Determination of Trace Amount of Ibutilide Fumarate in Pharmaceutical Manufacturing Environments

2009 ◽  
Vol 6 (1) ◽  
pp. 53-60
Author(s):  
M. Satya Babu ◽  
Prathama S. Mainkar ◽  
Y. Anjaneyulu
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Gradient Elution ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Chromatography Method ◽  
Test Concentration ◽  
Liquid Chromatography Method ◽  
Manufacturing Environments

A rapid and sensitive RP-HPLC method with UV detection at 227 nm for routine analysis of washed MLs (mother liquors) from equipment after manufacturing and thereby cleaning of ibutilide fumarate active pharmaceutical ingredient was developed. Chromatography was performed with mobile phase containing a mixture of aqueous 0.01 M potassium dihydrogen phosphate (KH2PO4) and acetonitrile. The gradient elution was developed for better and optimized results. The developed method was validated for precision which includes system precision and method precision, accuracy, intra-day and using different system and finally linearity studies from 0.4 to 150%. The method is ascertained to be having good repeatability and reproducibility. The %RSD for method precision (5 different preparations at test concentration) was observed to be 1.36, wherein the system precision (6 repeated injections of same preparation) was observed to be 0.33. The % recovery from ‘Accuracy’ studies yielded the recovery of 99-100% which indicates the capability of the method. The linearity of the method was studied right from 0.4 to 150% which shows the method is quite linear with a correlation coefficient of 0.9998. The proposed method was simple, highly sensitive, precise, and accurate.The retention time less than 15 min, indicated that the method is useful for routine testing of washed MLs from equipment after manufacturing and cleaning of ibutilide fumarate.

scholarly journals Development of a high-performance liquid chromatography method for simultaneously analyzing Guanosine 5’-monophosphate (GMP) and Inosine 5’-monophosphate (IMP) in food

2021 ◽  
Vol 4 (4) ◽  
pp. 298-306
Author(s):  
Dinh Hai Le ◽  
Thu Nguyen Thi ◽  
Trang Vu Thi ◽  
Thuy Le Thi ◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Food Products ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Food Matrix ◽  
Chromatography Method ◽  
Potassium Dihydrogen ◽  
Sample Preparation Procedure ◽  
Liquid Chromatography Method

This study aimed to develop a HPLC method to simultaneously analyze guanosine 5’-monophosphat (GMP) and inosine 5’-monophosphat (IMP) in food products. Sample preparation procedure was simple, fast. A C18 column (250 mm × 4.6 mm, 5 µm) was used as stationary phase, and a mixture of 10 mM potassium dihydrogen phosphate and 5 mM sodium heptanesulfonate was applied as mobile phase, and PDA detector at 250 nm. The method validation followed AOAC criteria. Selectivity, linearity (R2 > 0.999), recovery (IMP: 90.5 % - 102.8 %, GMP: 91.5 % - 103.9 %), repeatability (RSDR of IMP: 3.07 % and GMP: 2.83 %) were acceptable to determination GMP and IMP in food matrix under AOAC guidelines. LOD of GMP and IMP were of 2.32 and 2.77 mg/kg, respectively. This method was used to determination GMP, IMP in food products collected in Hanoi markets.

scholarly journals Method Development and Validation for Simultaneous Estimation of Benidipine Hydrochloride and Metoprolol Succinate in Tablet

2019 ◽  
Vol 9 (6-s) ◽  
pp. 28-33
Author(s):  
Dhaval M Patel ◽  
Deepa Patel ◽  
Advaita Patel ◽  
Avani Sheth ◽  
Utsav J Shah
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Chromatography Method ◽  
Metoprolol Succinate ◽  
Temperature Detection ◽  
Liquid Chromatography Method

Present work focusing in developing and validating a new high performance liquid chromatography method for estimation of Metoprolol Succinate and Benidipine Hydrochloride in their combine tablet dosage form. The method was performed on Shimadzu LC-20AT instrument using C18 (250 mm x 4.6 mm, 5 µm) Hypersil BDS Column and Potassium Dihydrogen Phosphate Buffer (pH 4.0): Methanol (65: 35% v/v) as mobile phase at ambient temperature. Detection was carried out at 269 nm. Concentration range 4-12 µg/ml for Benidipine Hydrochloride and 25-75 µg/ml for Metoprolol Succinate . The Percentage recovery of Benidipine Hydrochloride and Metoprrolol succinate was found to be 99.59% and 99.39 respectively. Correlation coefficient for Metoprolol succinate and Benidipine Hydrochloride was found 0.9995 and 0.9997 respectively. The Rt values for Metoprolol succinate and Benidipine Hydrochloride were found to be 3.4 and 5.9 min respectively. The method was validated according to the guidelines of International Conference on Harmonisation (ICH) and was successfully employed in the estimation of commercial formulations. Keywords:  Metoprolol Succinate, Benidipine Hydrochoride, HPLC, Mobile Phase,

scholarly journals Development and Validation of a Stability Indicating RP-HPLC Method for the Determination of Prucalopride succinate in Bulk and Tablet

2020 ◽  
pp. 166-174
Author(s):  
Sangameshwar B. Kanthale ◽  
Sanjay S. Thonte ◽  
Sanjay S. Pekamwar ◽  
Debarshi Kar Mahapatra
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Chromatography Method ◽  
Column Temperature ◽  
Stability Indicating ◽  
Variability Study

A very simple, precise, economical, accurate, robust, and reproducible reverse phase-high-performance liquid chromatography method along with stability indicating attributes has been developed for estimating of prucalopride succinate (PRU) in both bulk and tablet formulation (PRUVICT 2). The estimation of the solutes was performed on a Grace C18 column of dimension 150 mm × 4.6 mm, 5 μm. PRU was eluted with acetonitrile: 0.02 M potassium dihydrogen phosphate in the ratio of 20:80 v/v in a 10 min isocratic mode at a flow rate of 1 ml/min at 30°C column temperature and monitored at a wavelength of 277 nm. The retention time of PRU was found to be 5.416 minutes. The Q2b validation of the analytical method revealed good linearity over the concentration range 2–12 μg/mL for IVA with r2 of 0.999. The mean recovery % over the three tested ranges of 50%, 100%, and 150% were found to be 100.173%, 99.077%, and 98.575%, respectively. In intra-day variability study, the % RSDs was detected to be 0.754, 1.032, and 0.482 whereas the inter-day variability study demonstrated % RSDs of 0.797, 0.559, and 0.524, respectively. The acid, alkali, boiled water, hydrogen peroxide, dry heat, and UV radiations based stress studies presented the formation of a variety of characteristic degradation products. The developed analytical method may be employed for the routine analysis of PRU in bulk and tablet formulations.

HPLC DETERMINATION OF N-METHYLETHANOLAMINE IN DIPHENHYDRAMINE HYDROCHLORIDE DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 56-62
Author(s):  
A Anerao ◽  
◽  
V. Dighe ◽  
A Gupta ◽  
C. Patil ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Diphenhydramine Hydrochloride ◽  
Liquid Chromatography Method

N-Methylethanolamine is the side chain of the drug diphenhydramine hydrochloride. A sensitive high performance liquid chromatography method with pre-column derivatization was developed and validated for the determination of N-methylethanolamine impurity in diphenhydramine hydrochloride active pharmaceutical ingredient. HPLC method on column Cosmosil MS-II, C-18, 250 mm X 4.6 mm, particle size 5 μm with UV detector was used. The proposed method is specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.03 mg/g to 1.5 mg/g and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) as 0.01 mg/g and 0.03 mg/g, respectively, of the analyte. Accuracy was observed within 94.4% to 96.2%.

DEVELOPMENT AND VALIDATION OF HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF DEXTROMETHORPHAN HYDROBROMIDE AND QUINIDINE SULPHATE IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 35-40
Author(s):  
A. S. Bagde ◽  
V. V. Khanvilkar ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Dextromethorphan Hydrobromide

The present work describes a validated reverse phase high performance liquid chromatography (RPHPLC) method for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate in pharmaceutical dosage from. The drugs were resolved using Hemochrom Intsil C18-5U column (250×4.6) mm in isocratic mode with mobile phase methanol: water (0.08% diethylamine, 0.02% of glacial acetic acid and pH 4.4 adjusted with orthophosphoric acid) in the ratio of 70:30 V/V at a flow rate of 1.0 mL/min. Retention time of dextromethorphan hydrobromide and quinidine sulphate were 4.9±0.2 and 3.6±0.2, respectively, at 292nm. The above mentioned method was validated as per International Conference on Harmonization (ICH) guidelines. Linear responses were obtained in concentration ranges of 5-35 μg/mL for dextromethorphan hydrobromide and 4-16 μg/mL for quinidine sulphate, with correlation coefficient (r2) of 0.999 for both the drugs. A simple, selective, accurate, precise, robust and reliable RP-HPLC method thus developed and validated for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

scholarly journals HPLC-UV method for quantification of favipiravir in pharmaceutical formulations

2020 ◽  
Author(s):  
İbrahim Bulduk
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Potential Candidate ◽  
Column Temperature ◽  
Candidate Drug ◽  
System Suitability ◽  
Relative Standard

AbstractFavipiravir (FVP), a pyrazine analog, has shown antiviral activity against a wide variety of viruses. It is considered to be worth further investigation as a potential candidate drug for COVID-19. It is not officially available in any pharmacopoeia. A rapid, simple, precise, accurate, and isocratic high performance liquid chromatography (HPLC) method has been developed for routine quality control of favipiravir in pharmaceutical formulations. Separation was carried out by C18 column. The mobile phase was a mixture of 50 mM potassium dihydrogen phosphate (pH 2.3) and acetonitrile (90:10, v/v) at a flow rate of 1 mL min−1. The ultraviolet (UV) detection and column temperature were 323 nm, and 30 °C, respectively. The run time was 15 min under these chromatographic conditions. Excellent linear relationship between peak area and favipiravir concentration in the range of 10–100 μg mL−1 has been observed (r2, 0.9999). Developed method has been found to be sensitive (limits of detection and quantification were 1.20 μg mL−1 and 3.60 μg mL−1, respectively), precise (the interday and intraday relative standard deviation (RSD) values for peak area and retention time were less than 0.4 and 0.2%, respectively), accurate (recovery, 99.19–100.17%), specific and robust (% RSD were less than 1.00, for system suitability parameters). Proposed method has been successfully applied for quantification of favipiravir in pharmaceutical formulations.

LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF RELATED IMPURITIES OF LURASIDONE AND ITS FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (09) ◽  
pp. 41-48
Author(s):  
R. N Kachave ◽  
◽  
P. B. Mandlik ◽  
S. R. Nisal
Keyword(s):  
Method Development ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chromatography Method ◽  
Related Impurities ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
The Stability ◽  
Development And Validation

An RP-HPLC method was developed for the quantification of related impurities of lurasidone and its formulation. The chromatographic separation employs gradient elution using an Inertsil ODS C18 (150x4.6) mm, 5μm columns. Mobile phase consisting of solvent A-buffer (pH 3.0): methanol (90:10 %v/v) and solvent B-acetonitrile: water (80:20 % v/v) delivered at a flow rate of 1.0 mL/min. The analytes were detected and quantified at 210 nm using PDA. The method was validated as per ICH guidelines, demonstrating to be a simple, precise, selective, linear and accurate within the corresponding range of impurities of lurasidone. Linearity was observed in the concentration range of 2-6 µg/mL. The RT for Lurasidone was about 18.5 min and three known impurities at RRT about 0.15, 0.21 and 0.36. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under oxidative conditions. Degradation impurities did not interfere with the RT of drug. The peak purity obtained with the aid of PDA detection and satisfactory resolution between related impurities established the specificity of the determination. All these results provide the stability indicating capability of the method.

scholarly journals Quantitative Estimation of Sorafenib Tosylate Its Pure Form and in Its Tablet Formulation by RP-HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-3 ◽  
Author(s):  
R. Kalaichelvi ◽  
E. Jayachandran
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Composition ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Liquid Chromatography Method ◽  
Isocratic Mode

A simple, accurate, specific reverse-phase, high-performance liquid chromatography method has been developed for the determination of sorafenib tosylate in its pure form and its tablets. In this method, sorafenib tosylate was eluted by isocratic mode using a Phenomenex Luna C18 column by a mobile phase composition of acetonitrile and water in the ratio of 82.5 : 17.5, v/v. The flow rate was 1.5 mL/min. The eluted drug was monitored at 265 nm and the method was found to be linear from 5 to 80 μg/mL. The method was validated by linearity, precision, accuracy, LOD, and LOQ. The accuracy report denotes that there is not any interference of additives used in the formulation.

scholarly journals Stability-Indicating Method for Determination of Oxyphenonium Bromide and Its Degradation Product by High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1250-1257 ◽  
Author(s):  
Alaa EL-Gindy ◽  
Samy Emara ◽  
Heba Shaaban
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Order Rate Constant ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating Method ◽  
Oxyphenonium Bromide

Abstract A high-performance liquid chromatographic (HPLC) method was developed for determination of oxyphenonium bromide (OX) and its degradation product. The method was based on the HPLC separation of OX from its degradation product, using a cyanopropyl column at ambient temperature with mobile phase of acetonitrile25 mM potassium dihydrogen phosphate, pH 3.4 (50 + 50, v/v). UV detection at 222 nm was used for quantitation based on peak area. The method was applied to the determination of OX and its degradation product in tablets. The proposed method was also used to investigate the kinetics of the acidic and alkaline degradation of OX at different temperatures, and the apparent pseudo first-order rate constant, half-life, and activation energy were calculated. The pH-rate profile of the degradation of OX in Britton-Robinson buffer solutions within the pH range 212 was studied.

Sign in / Sign up

Export Citation Format

Share Document