A Validated Enantioselective HPLC Method for Determination of Ibuprofen Enantiomers in Bulk and Tablet Dosage Form

2016 ◽  
Vol 99 (3) ◽  
pp. 604-611 ◽  
Author(s):  
Hamed M El-Fatatry ◽  
Mokhtar M Mabrouk ◽  
Sherin F Hammad ◽  
Samah F El-Malla
Keyword(s):  
Chiral Stationary Phase ◽  
Dosage Form ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Enantioselective Resolution ◽  
Ibuprofen Enantiomers ◽  
Tablet Dosage ◽  
Interday Precision

Abstract A new chiral reversed-phase (RP)-HPLC method with UV detection was developed. Enantioselective resolution of ibuprofen (IBP) was achieved using (3R,4S)-4-(3,5-dinitrobenzamido)-3-(3-(trioxysilyl)-propyl)-1,2,3,4-tetrahydro-phenanthrene [(R,R)-Whelk-O2] chiral stationary phase (4.6 mm id × 250 mm, 10 μm) with a mobile phase composed of ethanol–water (30 + 70, v/v) containing 100 mM ammonium acetate at a flow rate of 1.3 mL/min using diode array detector at λ 220 nm. Calibration curves were linear over the concentration range of 20–180 μg/mL for both IBP enantiomers. Mean % recoveries ±SD of 99.74 ± 1.73 and 99.60 ± 0.93 were obtained for dexibuprofen (dex-IBP) and levoibuprofen (levo-IBP), respectively. Intra- and interday precision calculated as RSD, % were not more than 1.66% for dex-IBP and 1.93% for levo-IBP. The detection limits were 2.09 and 2.06 μg/mL for dex-IBP and levo-IBP, respectively. The method was successfully applied for the determination of dex-IBP in tablet dosage form.

scholarly journals A Validated Reversed-Phase HPLC Method for the Determination of Vildagliptin from Tablet Dosage Form

2013 ◽  
Vol 2 (3) ◽  
pp. 90-98 ◽  
Author(s):  
Rahima Khatun ◽  
Md Mirazzunnabi
Keyword(s):  
Dosage Form ◽  
Theoretical Plate ◽  
Cost Effective ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Buffer Solution ◽  
Column Temperature ◽  
Tablet Dosage

A simple, rapid, precise and cost effective method has been developed and validated for determination of Vildagliptin in pharmaceutical tablet dosage form. The chromatographic separation was carried out with Shimpack VP-ODS, 150 × 4.6 mm, 5?m analytical column and mobile phase containing 0.02M phosphate buffer (pH 4.6) and acetonitrile at the ratio (80:20% v/v). pH of the buffer solution was adjusted with orthophosphoric acid. The instrumental settings include flow rate 0.7 ml/min, column temperature at 25ºC and detector wavelength of 210nm using a photodiode array detector. Theoretical plate for Vildagliptin was 6219 and tailing factor was 1.38. DOI: http://dx.doi.org/10.3329/ijpls.v2i3.15455 International Journal of Pharmaceutical and Life Sciences Vol.2(3) 2013: 90-98

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF BAMIFYLLINE HYDROCHLORIDE IN TABLET DOSAGE FORM

2017 ◽  
Vol 9 (4) ◽  
pp. 76
Author(s):  
Panchumarthy Ravisankar ◽  
Shaheem Sulthana ◽  
Inturi Mary Thanuja ◽  
A. Dihitha Chowdary ◽  
J. Vyshnavi
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation ◽  
Tablet Dosage

Objective: The objective of the current study was to develop and validate a novel RP-HPLC method for determination of bamifylline hydrochloride in pharmaceutical dosage form.Methods: Chromatographic separation was conducted on Agilent technologies-1260 series with the G1311C quaternary pump, eclipse XDB C18 column (4.6 mm i.d. X 250 mm, 5 µm particle sizes) and equipped with photodiode array detector G1315D. Mobile phase consisted of methanol and acetonitrile were mixed in the ratio of 90:10 v/v, was used at a flow rate of 1 ml/min and detection wavelength was set at 263 nm.Results: The retention time for bamifylline hydrochloride was found to be 2.913 min. The calibration was linear (r2= 0.9996) in the concentration range of 2-10 µg/ml. The limit of detection and the limit of quantitation were found to be 0.4825 μg/ml and 1.4621 µg/ml respectively. Recovery of bamifylline hydrochloride in tablet formulation was observed in the range of 99.6-99.8 %. Percentage assay of bamifylline hydrochloride (Bamifix) was found to be 99.4 % w/w.Conclusion: Thus the novel proposed method for bamifylline hydrochloride was found to be feasible for the estimation of bamifylline hydrochloride in bulk as well as a pharmaceutical dosage form. 

scholarly journals Development of Simple and Robust RP-HPLC Method for Determination of Everolimus and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantitation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

FORCED DEGRADATION STUDIES OF OLMESARTAN MEDOXOMIL AND CHLORTHALIDONE: DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING RP‑HPLC METHOD

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (03) ◽  
pp. 39-45
Author(s):  
A Sherje ◽  
A. Sonalkar ◽  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Olmesartan Medoxomil ◽  
The United States ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Tablet Dosage

A reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of olmesartan medoxomil (OLME) and chlorthalidone (CHLOR) in tablet dosage form. The analysis was performed on Inertsil ODS C18 (250 x 4.6 mm, 5 μ) using KH2PO4 phosphate buffer (pH) and acetonitrile as mobile phase in the proportion of 60: 40 v/v at flow rate of 1.0 mL/min. Detection of drugs was carried out in isocratic mode using UV detector at 275 nm. The retention time of OLME and CHLOR was 13.9 ± 0.1 min. and 4.4 ± 0.5 min., respectively and the total run time was 20 min. The method was validated according to the requirements of the United States Pharmacopeia. The percentage recoveries was found to be in the range of 98.9 - 100.7%. The method was successfully applied to the assay of OLME and CHLOR in tablet dosage form.

HPLC METHOD DEVELOPMENT FOR ESTIMATION OF RAMELTEON IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (06) ◽  
pp. 20-23
Author(s):  
S Sahoo ◽  
◽  
P. K. Panda ◽  
S. K. Mishra
Keyword(s):  
Flow Rate ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Ich Guidelines ◽  
Hplc Method Development ◽  
Tablet Dosage ◽  
Good Agreement

A simple, fast, accurate and precise reverse phase HPLC method is developed and described for the determination of ramelteon in tablet dosage form. Chromatography was carried on an ODS column using a mixture of acetonitrile and phosphate buffer pH 7.0 (35:65 V/V) as the mobile phase at a flow rate of 1.0 mL/min with detection at 286 nm. The retention time of the drug was 7.7 min. The procedure was validated for linearity, precision, accuracy, and robustness. The developed method was validated for linearity from 50 to 150% which shows the method is quite linear with a correlation coefficient of 0.999, for precision which includes system precision, method precision, intraday and by another analyst on another day, and accuracy. The %RSD for system precision was observed to be 1.1, whereas the method precision was observed to be 0.2. The % recovery from ‘accuracy’ studies yielded the recovery of 99.7-101.5% which indicates the capability of the method, and finally for robustness that includes studies w.r.t. change in flow rate, the percentage of organic modifier and pH. As per ICH guidelines, method validation results are in good agreement. The proposed method was simple, sensitive, precise and accurate.

Stability Indicating Photodiode Array Detector Based Estimation of Dapagliflozin Propanediol Monohydrate in API and Tablet Dosage Form by RP-UPLC

2021 ◽  
pp. 4635-4639
Author(s):  
Ashok B. Patel ◽  
Ekta H. Vaghasiya ◽  
Amit R. Dudhatra ◽  
Amitkumar J. Vyas ◽  
Ajay I. Patel ◽  
...  
Keyword(s):  
Dosage Form ◽  
Active Pharmaceutical Ingredient ◽  
Array Detector ◽  
Column Temperature ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Acceptable Method ◽  
Photodiode Array ◽  
Tablet Dosage

Stability indicating RP-UPLC photo diode array detector based method for determination of Dapagliflozin propanediol monohydrate (DPM) in active pharmaceutical ingredient (API) and in tablet dosage form (5mg dapagliflozin) has been developed and validated on Bridge Ethylene Hybride (BEH) C18 column (50mm × 2.1 mm, 1.7µm). Mobile phase composition was water: acetonitrile (60:40 v/v), flow rate 0.5ml/min and detection carried out at 223nm at column temperature 30ºC. Chromatographic separation achieved within 2 min with retention time 0.77 min. Linearity of the method was found over the concentration range of 25-75µg/ml (R2 = 0.9977). The degradation was carried out in five different stress conditions. The developed method was able to resolve peak of API from all generated peaks. Sufficient degradation was achieved in the range of 5.25 to 12.31%. The peak purity is acceptable, Method validation was performed as per ICH guideline Q2(R1).

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

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