DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR RILPIVIRINE HYDROCHLORIDE IN BULK AND USE IN ANALYSIS OF PREPARED NANOSUSPENSION

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (04) ◽  
pp. 42-46
Author(s):  
Madhuri Manchala ◽  
◽  
Vijaya Sri Kanagala ◽  
Ganapath Vinay Jain
Keyword(s):  
Homogenization Method ◽  
Hplc Method ◽  
Array Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation ◽  
Tablet Dosage

A simple, precise, accurate and robust RP-HPLC-PDA method was developed and validated for the determination of rilpivirine hydrochloride in tablet dosage forms. Reverse-phase chromatography was performed on a BDS hypersil (250 mm × 4.6 mm, 6 μm) column of Waters HPLC with Empower software and with a photodiode array detector. Methanol: acetonitrile: water 80:13.5:6.5 (v/v) was used as the mobile phase at a flow rate of 1 mL min-1 with PDA detection at 306 nm. Rilpivirine hydrochloride nanosuspension was prepared by using an ultrasonic homogenization method. Linearity was observed in the concentration range of 0.1–10 μg mL-1 with regression equation y = 508856X+46908 (R2 = 0.9998). The method was validated as per ICH guidelines. The RSD for intra-day (1.31- 0.67) and inter-day (1.69-1.59) precision was found to be less than 2%. The developed method is simple, precise and robust for the determination of rilpivirine hydrochloride and is successfully applied for the nanosuspension.

Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil

2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu
Keyword(s):  
Analytical Method ◽  
Anhydrous Sodium Sulfate ◽  
Hplc Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Precision And Accuracy ◽  
Hplc Grade Acetonitrile ◽  
Development And Validation

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.

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.

scholarly journals Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

PLoS ONE ◽  
2021 ◽  
Vol 16 (3) ◽  
pp. e0244951
Author(s):  
Hany W. Darwish ◽  
Nesma A. Ali ◽  
Ibrahim A. Naguib ◽  
Mohamed R. El Ghobashy ◽  
Abdullah M. Al-Hossaini ◽  
...  
Keyword(s):  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Alkaline Conditions ◽  
Development And Validation

A reliable, selective and sensitive stability-indicating RP-HPLC assay was established for the quantitation of bromazepam (BMZ) and one of the degradant and stated potential impurities; 2-(2-amino-5-bromobenzoyl) pyridine (ABP). The assay was accomplished on a C18 column (250 mm × 4.6 mm i.d., 5 μm particle size), and utilizing methanol-water (70: 30, v/v) as the mobile phase, at a flow rate of 1.0 ml min-1. HPLC detection of elute was obtained by a photodiode array detector (DAD) which was set at 230 nm. ICH guidelines were adhered for validation of proposed method regarding specificity, sensitivity, precision, linearity, accuracy, system suitability and robustness. Calibration curves of BMZ and ABP were created in the range of 1–16 μg mL-1 with mean recovery percentage of 100.02 ± 1.245 and 99.74 ± 1.124, and detection limit of 0.20 μg mL-1 and 0.24 μg mL-1 respectively. BMZ stability was inspected under various ICH forced degradation conditions and it was found to be easily degraded in acidic and alkaline conditions. The results revealed the suitability of the described methodology for the quantitation of the impurity (ABP) in a BMZ pure sample. The determination of BMZ in pharmaceutical dosage forms was conducted with the described method and showed mean percentage recovery of 99.39 ± 1.401 and 98.72 ± 1.795 (n = 6), respectively. When comparing the described procedure to a reference HPLC method statistically, no significant differences between the two methods in regard to both accuracy and precision were found.

Method Development and Validation for Estimation of Istradefylline in Tablet Dosage form by RP-HPLC

2021 ◽  
pp. 4767-4772
Author(s):  
Krishna Kishore Adireddy ◽  
Srinivasa Rao Baratam ◽  
Nagarjuna Hari Pratap S
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Solution Stability ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of Istradefylline in table dosage form. Chromatographic analysis of the drug was achieved on Shimadzu HPLC comprising of LC- 20 AD binary gradient pump, a variable wavelength programmable SPD-20A detector and SCL system controller. C18G column (250 mm x 4.6 mm, 5 μ) as stationary phase with mobile phase consisting of 0.1 % orthophosphoric acid and acetonitrile in the ratio of 30: 70 v/v. The method showed a good linear response in the concentration range of 10-90 μg/ml with correlation coefficient of 0.9993. The flow rate was maintained at 1.0 ml/min and detection was carried out at 246 nm. The retention time was 3.125 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, solution stability, selectivity and sensitivity. The results obtained in the study were within the limits of ICH guidelines and hence this method can be used for the determination of istradefylline in tablet formulation.

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 and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Sofosbuvir, Velpatasvir, and Voxilaprevir in Tablet Formulation

2020 ◽  
pp. 7-14
Author(s):  
Deepthi R ◽  
Gowri Sankar D
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Solution Stability ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Optimized Conditions

Objective: The present study aimed to develop a stability-indicating reverse-phase high performance-liquid chromatography (RP-HPLC) method for the estimation of Sofosbuvir, Velpatasvir, and Voxilaprevir in tablet dosage form and validated in accordance with ICH guidelines. Methods: The optimized conditions for the developed RP-HPLC method are Agilent C18 (250 mm×4.6mm, 5μ) column maintained at 30ºC with a mobile phase consisting of Buffer(0.1%OPA) and Acetonitrile taken in the ratio 55:45%v/v on isocratic mode at flow rate 1.0ml/min. The sample was detected at 220 nm. Results: The retention time of Sofosbuvir, Velpatasvir, and Voxilaprevir was found to be 2.17, 2.731 and 3.55 min respectively. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability.

Simultaneous Determination of Co-administrated Deflazacort, Aprepitant and Granisetron in Dosage Forms and Spiked Human Plasma by RP-HPLC/PAD

2019 ◽  
Vol 57 (9) ◽  
pp. 790-798 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Soheir Alweshahy ◽  
Dalia A Elshabasy ◽  
Nadia F Youssef
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Array Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array

Abstract A selective reversed phase high performance liquid chromatography/photodiode array detector (RP-HPLC/PAD) method has been developed for simultaneous determination of the three co-administrated deflazacort, aprepitant and granisetron drugs used with chemotherapy. The three cited drugs have been chromatographed on C18 column using a mobile phase consisting of acetonitrile–0.2% v/v triethylamine (80:20 v/v, pH of 6.6 ± 0.05) with isocratic elution and monitored by photodiode array at 220 nm. International conference on harmonization (ICH) guidelines were followed to validate the developed method. Successful application of the developed method was assessed by the simultaneous determination of the studied drugs in pure forms, dosage forms and plasma samples in the ranges of 0.2–20, 0.4–40 and 0.2–20 μg/mL for deflazacort, aprepitant and granisetron, respectively.

scholarly journals Stability indicating RP HPLC method for determination of levitiracetam in pharmaceutical formulation

2013 ◽  
Vol 1 (04) ◽  
pp. 45-54 ◽  
Author(s):  
M. Krishna Chaitanya Prasad ◽  
G. Vidhya Sagar ◽  
P. Sudhakar
Keyword(s):  
Stress Testing ◽  
Hplc Method ◽  
Chromatographic Separations ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array ◽  
Standard Calibration ◽  
Tablet Dosage

The article reports on a development of RP-HPLC method for the quantitative determination of Levetiracetam in tablet dosage forms. The chromatographic separations were performed using Phenomenex_ C18 (250 mm x 4.6 mm i.d, 5 μm particle size) column at 40 ºC temperatures. The optimum mobile phase consisted of methanol, water and acetonitrile in the ratio of 30:10:60. Auto sampler 20 μl was used and kept at 15 ºC temperature. Analysis was done with flow rate of 1.0 ml/min at 212 nm (_ max of Levetiracetam) wavelength by using photodiode array (PDA) detector. The drug was analyzed for acid, alkaline, oxidative, hydrolytic, photolytic and thermal degradation studies. The standard calibration curve was plotted for the drug and results showed that the drug was linear (r2 = 0.999) in the concentration range between 0.01 – 1.5 μg/ml. The results of stress testing undertaken according to the International Conference on Harmonization (ICH) guidelines reveal that the selected method is selective and stability-indicating for determination of levitiracetam in pharmaceutical formualtion.

scholarly journals Development and Validation of a Column High-Performance Liquid Chromatography Method for Quantification of Ganaphaliin A and B in Inflorescences of Gnaphalium liebmannii Sch. Bp ex Klatt

2011 ◽  
Vol 94 (4) ◽  
pp. 1076-1081 ◽  
Author(s):  
Fernando Rodríguez-Ramos ◽  
Víctor H Sánchez-Estrada ◽  
Alejandro Alfaro-Romero ◽  
Gabriela Rubí Tapia-Álvarez ◽  
Andrés Navarrete
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Raw Material ◽  
Array Detector ◽  
Chromatography Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatography Method ◽  
Development And Validation

Abstract An HPLC method was developed for the simultaneous determination of gnaphaliin A and B, active compounds of Gnaphalium liebmannii Sch. Bp ex Klatt. The HPLC separation was performed on an Inertsil ODS-3 (150 × 4.6 mm id, 5 μm) RP C18 column operated at 40°C; the isocratic mobile phase was 0.02% aqueous orthophosphoric acid– methanol–acetonitrile (50 + 30 + 20, v/v/v), with a run time of 20 min and flow rate of 1.5 mL/min. Detection with a photodiode array detector (PDAD) was at 270 nm. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ for gnaphaliin A and B were found to be in the range of 0.4–0.5 and 1.0–1.4 μg/mL, respectively. This is the frst report of an analytical method developed for the quantitative analysis of flavones from Gnaphalium species by HPLC-PDAD with applications for raw material and commercial products.

scholarly journals RP-HPLC-DAD method for determination of olmesartan medoxomil in bulk and tablets exposed to forced conditions

2010 ◽  
Vol 60 (1) ◽  
pp. 13-24 ◽  
Author(s):  
Ritesh Sharma ◽  
Shyam Pancholi
Keyword(s):  
Degradation Products ◽  
Olmesartan Medoxomil ◽  
Array Detector ◽  
Drug Degradation ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Tablet Dosage

RP-HPLC-DAD method for determination of olmesartan medoxomil in bulk and tablets exposed to forced conditionsA simple, sensitive and precise RP-HPLC-DAD method was developed and validated for the determination of olmesartan medoxomil (AT-II receptor blocker) in the presence of its degradation products. Olmesartan medoxomil and all the degradation products were resolved on a C18column with the mobile phase composed of methanol, acetonitrile and water (60:15:25,V/V/V, pH 3.5 by orthophosphoric acid) at 260 nm using a photodiode array detector. The method was linear over the concentration range of 1-18 μg mL-1and precise with RSD < 1 % in intra- and inter-day study. Excellent recoveries of 99.3 ± 0.9 to 100.8 ± 1.2% proved the accuracy of the method. Developed method was specific, as indicated by chromatographic resolution > 2.0 for each peak and sensitive withLOD0.03 μg mL-1andLOQ0.1 μg mL-1. The method was used to study the drug degradation behavior under forced conditions. Four degradation products (DP-I, II, III, IV) were formed during the degradation study in 0.1 mol L-1HCl whereas only DP-I, II and III were formed in water, 0.01 mol L-1NaOH and 3% H2O2. No significant thermal or photolytic degradation was observed in solid drug. The method was applied successfully for the assay of olmesartan medoxomil in the tablet dosage form.

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