scholarly journals Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Lenalidomide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 35 (1) ◽  
pp. 140-149 ◽  
Author(s):  
Somana Siva Prasad ◽  
G. V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Stability Robustness ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Limit Of Quantitation ◽  
Successful Separation ◽  
Quality By Design Approach

In this study, a novel, simple and precise RP-HPLC method has been developed for the quantitative analysis of Lenalidomide (LLM) in pharmaceutical formulations using analytical quality by design approach. An X-bridge-C18 column (150 mm × 4.6 mm × 3.5 µ) with mobile phases containing a Potassium dihydrogen orthophosphate anhydrous buffer and methanol in the ratio of (90:10 v/v) and (35:65 v/v) are used for the estimation of LLM and its degradation products. The flow rate of 0.8 mL/min is maintained and all degradation studies are performed at 210 nm using photodiode array (PDA) detector. Method Validation is carried out according to International Council for Harmonisation (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful separation of LLM and its impurities in the pharmaceutical dosage formulations.

scholarly journals RP-HPLC Estimation of Bumetanide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (10) ◽  
pp. 2215-2221
Author(s):  
P. Suresh Kumar ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Fixed Dose ◽  
Array Detector ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation

A novel and simultaneous stability indicating RP-HPLC method has been developed for quantitative analysis of bumetanide in fixed dose pharmaceutical formulations. Bumetanide and its degradation products are well separated by the Discovery C18, 250 × 4.6 mm, 5 μm column as a stationary phase and (50:50 v/v) of 0.1 % o-phthalaldehyde and acetonitrile as a mobile phase. All the compounds are monitored using photodiode array detector at 254 nm with an isocratic method and the flow rate of 1.0 mL/min was maintained. Validation of method was performed as per International Council for Harmonization (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) were evaluated. The linearity of the proposed method was found to be 0.315-1.875 μg/mL for bumetanide and its impurities. The developed method is more economical and suitable for laboratory use because of solvent consumption is very less. Hence, the developed method can be used for the determination of bumetanide and its impurities in drug product stability studies and pharmaceutical formulations.

scholarly journals Fasten, simple, and specific stability of the avant-garde RP-HPLC method for estimation and validation of nystatin in pharmaceutical formulations

2019 ◽  
Vol 10 (4) ◽  
pp. 3717-3727
Author(s):  
Dawood CH. Al-Bahadily ◽  
Rasool Chaloob ◽  
Kulood H. Oudah ◽  
H. N. K. AL-Salman ◽  
Falah Hassan Shari ◽  
...  
Keyword(s):  
Flow Rate ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Avant Garde ◽  
Rp Hplc ◽  
Specificity And Sensitivity ◽  
Stress Degradation ◽  
The Stability

In this study, a simple and reliable stability-indicating RP-HPLC method was developed and validated for the analysis of Nystatin in the pharmaceuticals. The chromatographic separation was performed in the isocratic mode on an Ion Pac column; Arcus EP‑C18; 5μm, 4.6×250 mm, 30 °C) using a mobile phase consisting of ammonium acetate 0.05 M buffer/ Methanol mixture (30:70) and a flow-rate of 1.0 mL/min with UV detection at 305 nm. The flow rate was set at 1.0 mL/min. The HPLC analysis method was validated in terms of linearity, precision, accuracy, specificity, and sensitivity, according to International Conference on Harmonization (ICH) guidelines. The results indicated that the retention time was 8 min, and no interferences were observed from the formulation excipients and stress degradation products.  The specificity, linearity, precision, accuracy, LOD, and LOQ of the method were validated. The method was linear over the range of 5–500 μg/mL with an acceptable correlation coefficient (R2 = 0.9996). The method’s limit of detection (LOD) and quantification (LOQ) were 0.01 and 0.025 μg/mL, respectively. The results indicate that this validated method can be used as an alternative method for the assay of nystatin. This validated HPLC method could be used for routine analysis, quality control, and the stability of analysis of Nystatin formulations.

VALIDATION OF PROPOSED RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF FENPIVERINIUM BROMIDE AND PITOFENONE HCL

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (07) ◽  
pp. 39-45
Author(s):  
S.V Nagpure ◽  
◽  
S.V Deshmane ◽  
K.R. Biyani
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Diammonium Hydrogen

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of fenpiverinium bromide and pitofenone HCl. Separation of the drug was achieved on a reverse phase Thermo Kromasil C18 Column. The method showed a linear response for concentration in the range of 1.2-2.8μg/ml for FVB 6-14 μg/ml for PFH using diammonium hydrogen orthophosphatee buffer pH 7.2: acetonitrile as the mobile phase in the ratio of 55:45, v/v with detection at 220 nm with a flow rate of 1 ml/min and retention time was 3.77min and 7.45 min for FVB and PFH respectively. The method was statistically validated for linearity, accuracy, precision and selectivity.The limit of detection and limit of quantitation was 0.0654 µg/ml and 0.1982 µg/ml for FVB and 0.0927 µg/ml and 0.281 µg/ml for PFH, respectively. In quantitative and recovery studies, % RSD was found less than 2. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis of fenpiverinium bromide and pitofenone HCl in pharmaceutical formulations.

scholarly journals A Validated RP-HPLC Method for the Estimation of Quetiapine in Bulk and Pharmaceutical Formulations

2010 ◽  
Vol 7 (s1) ◽  
pp. S261-S266 ◽  
Author(s):  
D. Suneetha ◽  
A. Lakshmana Rao
Keyword(s):  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Detector Response ◽  
Control Analysis ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
The Mean

A new, simple, specific, sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of quetiapine in bulk and pharmaceutical formulations. Quetiapine was chromatographed on a reverse phase C18Waters column (75x4.6 mm I.D., particle size 3.5 μm) in a mobile phase consisting of phosphate buffer (pH 3.0 adjusted with orthophosphoric acid) and acetonitrile in the ratio 40:60 v/v. The mobile phase was pumped at a flow rate of 0.8 mL/min with detection at 291 nm. The detector response was linear in the concentration of 20-120 μg/mL. The limit of detection and limit of quantitation was found to be 0.2 and 0.75 μg/mL, respectively. The intra and inter day variation was found to be less than 1%. The mean recovery of the drug from the solution was 99%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of quetiapine in bulk and pharmaceutical formulations.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

scholarly journals Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Codeine Phosphate and Chlorpheniramine Maleate from Their Combined Liquid Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Ramakrishna Kommana ◽  
Praveen Basappa
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Codeine Phosphate ◽  
Chlorpheniramine Maleate ◽  
Combination Drug ◽  
Stability Indicating ◽  
Rp Hplc

The present paper describes the development of quick stability indicating RP-HPLC method for the simultaneous estimation of codeine phosphate and chlorpheniramine maleate in the presence of its degradation products, generated from forced degradation studies. The developed method separates codeine phosphate and chlorpheniramine maleate in impurities/degradation products. Codeine phosphate and chlorpheniramine maleate and their combination drug product were exposed to acid, base, oxidation, dry heat, and photolytic stress conditions, and the stressed samples were analysed by proposed method. The proposed HPLC method utilizes the Shimadzu HPLC system on a Phenomenex C18 column (, 5 μ) using a mixture of 1% o-phosphoric acid in water : acetonitrile : methanol (78 : 10 : 12) mobile phase with pH adjusted to 3.0 in an isocratic elution mode at a flow rate of 1 mL/min, at 23°C with a load of 20 μL. The detection was carried out at 254 nm. The retention time of codeine phosphate and chlorpheniramine maleate was found to be around 3.47 min and 9.45 min, respectively. The method has been validated with respect to linearity, robustness, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The developed validated stability indicating HPLC method was found to be simple, accurate, and reproducible for the determination of instability of these drugs in bulk and commercial products.

scholarly journals Development and Validation of RP-HPLC Method for Quantitative Estimation of Vinpocetine in Pure and Pharmaceutical Dosage Forms

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
Subrata Bhadra ◽  
Sreedam Chandra Das ◽  
Sumon Roy ◽  
Shamsul Arefeen ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Dosage Forms ◽  
Hplc Method ◽  
Array Detector ◽  
Acetate Solution ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Quality Control Tool

A simple, precise, specific, and accurate reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for determination of vinpocetine in pure and pharmaceutical dosage forms. The different analytical performance parameters such as linearity, accuracy, specificity, precision, and sensitivity (limit of detection and limit of quantitation) were determined according to International Conference on Harmonization ICH Q2 (R1) guidelines. RP-HPLC was conducted on Zorbax C18 (150 mm length × 4.6 mm ID, 5 μm) column. The mobile phase was consisting of buffer (containing 1.54% w/v ammonium acetate solution) and acetonitrile in the ratio (40 : 60, v/v), and the flow rate was maintained at 1.0 mLmin−1. Vinpocetine was monitored using Agilent 1200 series equipped with photo diode array detector (λ = 280 nm). Linearity was observed in concentration range of 160–240 μgmL−1, and correlation coefficient was found excellent (R2 = 0.999). All the system suitability parameters were found within the range. The proposed method is rapid, cost-effective and can be used as a quality-control tool for routine quantitative analysis of vinpocetine in pure and pharmaceutical dosage forms.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

Validated RP-HPLC method for the estimation of Amiloride and hydrochlorothiazide in combined tablet dosage form

2021 ◽  
pp. 207-211
Author(s):  
R. Anantha Kumar ◽  
G. Raveendr Babu ◽  
Sowjanya M. ◽  
Ramayyappa M.
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Tablet Dosage ◽  
Liquid Chromatographic

The aim of this work is to build up a fast, exact, precise and touchy reverse phase liquid chromatographic method for the synchronous assessment of amiloride and hydrochlorothiazide in tablet dose structure. The chromatographic strategy was normalized utilizing Hypersil ODS segment (250×4.6mm, 5μm molecule size) with UV discovery at 210nm and stream pace of 1ml/min. The portable stage includes phosphate buffer (pH acclimated to 2.5 with dilute Ortho Phosphoric acid) and acetonitrile in the proportion of 60:40 v/v. The linearity of proposed technique was examined in the scope of 5-30μg/ml (R²=0.999) for amiloride and 50-300μg/ml (R²=0.999) for Hydrochlorothiazide appropriately. The limit of detection (LOD) was discovered to be 0.10μg/ml and 0.40μg/ml for Amiloride and Hydrochlorothiazide appropriately. The limit of quantitation (LOQ) was discovered to be 0.30μg/ml and 1.20μg/ml for Amiloride and Hydrochlorothiazide separately. The retention times of Amiloride and Hydrochlorothiazide were found to be 3.258min and 2.383min separately. The technique was truly recommended and %RSD was found to be under 2 demonstrating serious level of exactness and accuracy. Subsequently proposed strategy can be effectively evaluated for the synchronous assessment of Amiloride and Hydrochlorothiazide in promoted formulations.

Sign in / Sign up

Export Citation Format

Share Document