scholarly journals QUANTIFICATION OF BILASTINE AND MONTELUKAST COMBINATION IN FORMULATIONS UTILIZING LIQUID CHROMATOGRAPHY: STABILITY STUDIES

2021 ◽  
pp. 210-215
Author(s):  
KANCHARLA VIJAYALAKSHMI ◽  
BETHAPUDI SAMUEL ANAND ANDREWS ◽  
BOLINENI NAGESWARA RAO
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Mobile Phase ◽  
Tablet Formulation ◽  
Uv Detection ◽  
Stability Studies ◽  
Stability Indicating ◽  
Quantitation Limit ◽  
Rp Hplc

Objective: We have developed a “stability-indicating RP-HPLC” procedure for the Bilastine (BLS) and montelukast (MTL) analysis of tablets. Methods: The quantification of BLS and MTL combination was implemented utilising a Waters column (C18, 5 μm, 250 mm and 4.6 mm). Isocratic mobile phase had 60% volume KH2PO4 of 0.1M strength with pH 4.2 units and 40% volume methanol at a flow with 1.0 ml/min speed. UV detection at 232 nm was done to examine BLS and MTL. Stability experiments of BLS and MTL under distinctive environments of stress were also performed. Results: The BLS and MTL were eluted at 1.810 min and 2.551 min, respectively. The responses were found to be linear for the concentration ranges of 10-30 µg/ml (BLS) and 5-15 µg/ml (MTL). Percent comparative standard deviance for precision was 0.331% (BLS) and 0.486% (MTL). Percent assay for accuracy was 98.96% (BLS) and 99.00% (MTL). The detection limit and quantitation limit measures for BLS were 0.018 µg/ml and 0.059 µg/ml, respectively, while for MTL it was 0.024 µg/ml and 0.081 µg/ml, respectively. Robustness studies authorized that the method is robust with percent comparative standard deviance of a highest 1.950%. Conclusion: The developed “stability-indicating RP-HPLC” procedure for the BLS and MTL analysis is simple, sensitive, precise, specific and robust, making it appropriate to the assessment of BLS and MTL in a tablet formulation.

scholarly journals New stability indicating RP-HPLC-PDA method for determination of mifepristone in bulk and tablet formulation

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Mohammad Mojeeb Gulzar Khan ◽  
Mohammad Faizan Saadique Deshmukh ◽  
Sandip Dinkar Firke ◽  
Abdul Talib Abdul Wahab ◽  
Mohan Ganpatrao Kalaskar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Forced Degradation ◽  
Established Method ◽  
Potassium Dihydrogen ◽  
Stability Indicating ◽  
Quantitation Limit ◽  
Rp Hplc

Abstract Background Mifepristone is progestational and glucocorticoid hormone antagonist. The objective of this study is to develop simple and economical stability indicating RP-HPLC method for the determination of mifepristone in bulk and tablet formulation. Result The chromatographic separation was achieved on Qualisil BDS C8 column with mobile phase containing of mixture of Buffer (Potassium dihydrogen ortho phosphate, pH to 3.0 with ortho phosphoric acid) and Organic Solvent (Acetonitrile) 60:40 v/v pumped at flow rate 0.6 mL min−1. The detection of elute was performed using PDA detector at 305 nm. Mifepristone was eluted at 8.67 min. According to international conference on harmonization Q2(R1) guideline, method was validated and shows satisfactory results for accuracy, precision, linearity, ruggedness, robustness, detection limit, quantitation limit. The method indicated to be linear in the series of concentration 3–18 µg mL−1, and correlation coefficient was 0.9997. In acidic, basic, oxidative, thermal, photolytic forced degradation conditions, the peak of degradation product was clearly and well separated from drug peak without any interference in quantitative analysis. This represents stability indicating nature of established method. Conclusion The established RP-HPLC method is simple, accurate, specific, precise, robust, rugged, sensitive, and economical in nature which can be utilized for routine analysis of mifepristone in bulk and pharmaceutical formulation.

scholarly journals Analysis of some pharmaceuticals in the presence of their synthetic impurities by applying hybrid micelle liquid chromatography

2020 ◽  
Vol 18 (1) ◽  
pp. 377-390
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba
Keyword(s):  
Liquid Chromatography ◽  
Sodium Dodecyl Sulfate ◽  
Phosphoric Acid ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Uv Detection ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Amino Phenol ◽  
The Stability

AbstractA stability-indicating hybrid micelle liquid chromatography accompanied by UV detection was developed for the simultaneous analysis of either paracetamol (PCA) or pseudoephedrine hydrochloride (PSU) with their synthetic impurities. Mixture I contains PCA with p-amino phenol and p-nitro phenol, while mixture II involves the estimation of PSU with benzaldehyde and benzoic acid. Both mixtures were separated using a C18 column that was thermostatically maintained at 40°C and operating under a flow rate of 1.5 mL/min, applying UV detection at 240 nm for mixture I and 220 nm for mixture II. In both cases, the mobile phase consisted of 0.1 M sodium dodecyl sulfate, acetonitrile, and triethylamine (90:10:0.3, v/v/v) and adjusted to pH 4 (mixture I) or pH 3.7 (mixture II) using 2.0 M O-phosphoric acid. The proposed method was validated and successfully applied to assay different pharmaceuticals containing PCA or PSU. Moreover, the stability-indicating nature of the proposed method was proved through applying photolytic degradation procedures for PCA.

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.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF ROSUVASTATIN CALCIUM AND CLOPIDOGREL BISULFATE IN PHARMACEUTICAL DOSAGE FORM BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2020 ◽  
pp. 84-90
Author(s):  
AWDHUT PIMPALE ◽  
RAJENDRA KAKDE
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Simultaneous Estimation ◽  
Stability Indicating ◽  
Clopidogrel Bisulfate ◽  
Rp Hplc ◽  
Development And Validation

Objective: The present work was focused on the development and validation of reversed-phase high-performance liquid chromatography (RP-HPLC) method which is simple, rapid, precise, accurate, sensitive, economical, and stability-indicating for the quantification of rosuvastatin (RSV) calcium and clopidogrel bisulfate (CLO) in bulk and tablet formulation. Methods: The separation was attained on RP Princeton (C18) column with dimensions (250 mm × 4.6 mm, 5 μ) employing buffer which is a mixture of water (pH 3.0, adjusted with orthophosphoric acid), and methanol in the ratio (20:80) v/v as mobile phase, at flow rate 1.0 ml/min and detection was carried out at wavelength 240 nm. The retention time under the optimized condition of RSV calcium and CLO was found to be 2.844 min and 4.388 min, respectively. Results: The linearity of the method was demonstrated in the concentration range of 6–16 µg/ml and 45–120 µg/ml for RSV calcium and CLO with a correlation coefficient (r2) of 0.9999 and 0.9996, respectively. The percentage relative standard deviation was ˂2% and percentage recovery was found to be 100.12–101.37% and 99.72–101.09% for RSV calcium and CLO, respectively. Assay of marketed tablet formulation was found to be 98.99% and 99.92%, respectively. Conclusion: The developed RP-HPLC method was found to be simple, specific, sensitive, rapid, linear, accurate, precise, and economical and could be used for regular quality control of RSV calcium and CLO in bulk and tablet formulations.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ROSUVASTATIN CALCIUM IN BULK AND TABLET FORMULATION BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 251-256
Author(s):  
SAILAJA B ◽  
SRAVANA KUMARI K
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Development And Validation ◽  
Rosuvastatin Calcium

Objective: The present work was focused on the development and validation of reverse-phase high-performance liquid chromatography (RP-HPLC) method which is simple, rapid, precise, accurate, sensitive, economical, and stability indicating for the quantitation of rosuvastatin calcium in bulk and tablet formulation. Methods: The separation was attained on Waters Symmetry C18 column with dimensions 150×4.6 mm, 5 mm particle size employing 0.1% orthophosphoric acid buffer:acetonitrile in the ratio of 55:45% v/v as mobile phase, which was pumped at a rate of 1.0 ml/min and detected at a wavelength of 241 nm. Results: The linearity of the method was demonstrated in the concentration range of 2–12 μg/ml for rosuvastatin calcium with a correlation coefficient (r2) of 0.999, percentage drug recovery was found to be 100.22–101.16%, and percentage relative standard deviation <2. Limit of detection and limit of quantitation values were found to be 0.013 μg/ml and 0.042 μg/ml, respectively, and assay of marketed tablet formulation was found to be 99.76%. Conclusion: The developed RP-HPLC method was found to be simple, specific, sensitive, rapid, linear, accurate, precise, and economical and could be used for regular quality control of rosuvastatin calcium in bulk and tablet formulation.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE ESTIMATION OF LEDIPASVIR IN BULK AND TABLET DOSAGE FORM

2019 ◽  
pp. 326-331
Author(s):  
MINAL R GHANTE ◽  
SANJAY D SAWANT ◽  
AMOLDEEP SHINDE ◽  
SHITAL GODSE ◽  
VANDANA S NIKAM
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

Objective: The objective of this study was to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the estimation of ledipasvir (LDP) in bulk and tablet formulation. Methods: Stability-indicating RP-HPLC method was developed and validated for the estimation of LDP in bulk and tablet formulation. RP-HPLC was carried out on HiQ SiL C18 columns (250 mm × 4.6 mm, 5 μ particle size) using mobile phase acetonitrile:1 mM ammonium acetate buffer in the ratio of 90:10 v/v at a flow rate of 1 ml/min. The analytes were monitored using MD 2010 PDA detector at 333 nm. Results: The retention time was found to be 3.843 min. The proposed method was found to be having linearity in the concentration range of 5–30 μg/ml. The number of theoretical plates obtained was 4236.50 which indicate the efficient performance of the column. The limit of detection was 0.305 μg/ml and limit of quantification was 0.923 μg/ml, which indicate the sensitivity of the method; the high percentage recovery indicates that the proposed method is highly accurate. The developed method has been validated according to the ICH guidelines and found to be simple, specific, precise, and accurate. Conclusion: The proposed method is precise, accurate, and stability indicating. Therefore, the proposed method can be used for routine quality control and analysis of LDP during stability studies in bulk samples and tablet dosage forms.

scholarly journals A Validated Stability Indicating RP-HPLC Method for Quantification of Cilnidipine in Bulk and in Tablet Dosage Form

2021 ◽  
Vol 37 (5) ◽  
pp. 1167-1177
Author(s):  
Rameshwar Gholve ◽  
Sanjay Pekamwar
Keyword(s):  
Detection Limit ◽  
Dosage Form ◽  
Hplc Method ◽  
Drug Substance ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quantitation Limit ◽  
Rp Hplc ◽  
The Mean ◽  
Tablet Dosage

A stability indicating RP-HPLC method has been developed for quantification of Cilnidipine in bulk and in tablet dosage form. The chromatographic analysis was accomplished at ambient temperature on Xttera RP18 (100 x 4.6 mm, 3.5 µm) column and 1 mL/min flow rate by using Eluent composed of 10 mM phosphate buffer pH 2.6 with Acetonitrile (300:700, v/v). The UV detection at the wavelength of 240 nm was carried out using 20 µL injection volume. The Cilnidipine retention time was found to be 3.029 min. The method in the range of 40.0573 – 120.1719 µg/mL was found to be linear (R2 = 0.999) with a detection limit and quantitation limit of 1.2038 and 3.6478 μg/mL, respectively. The mean recovery % over the three tested levels of 50, 100, and 150% were found to be 98.74, 99.60, and 98.23%, respectively. The mean % assay of 99.29 for method repeatability and 98.82 for intermediate precision were found with % RSD of 0.68 and 0.31, respectively. Cilnidipine drug substance and their product exposed to acid, alkali, oxidative, thermal, photolytic, and humidity stress conditions. The acid, alkali, and photolytic induced stress studies signifying the formation of a variety of degradants and their peaks were well resolved from that of active analyte peak. Hence, it is recommended that the Cilnidipine drug substance, as well as drug product, should be store in a tightly closed container protected from light. The method as per ICH guidelines was validated for specificity, linearity, detection limit, quantitation limit, precision, accuracy, robustness, solution stability, and can be effectively used for routine analysis.

scholarly journals STABILITY INDICATING REVERSE-PHASE HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF TELMISARTAN AND BENIDIPINE HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (5) ◽  
pp. 342
Author(s):  
Majan Naim ◽  
Aejaz Ahmed ◽  
Khan Gj
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Development And Validation

 Objective: Development and validation of stability indicating reverse-phase high- performance liquid chromatography (RP-HPLC) method for simultaneous estimation of telmisartan (TEL) and benidipine hydrochloride (BND) in pharmaceutical dosage form.Methods: Reverse phase chromatography was selected because of its suggested use for ionic and moderate to non-polar compounds. Reverse phase chromatography is simple, suitable, better regarding efficiency, stability, and reproducibility. C18 column, a 250×4.6 mm column of 5.0 μm particle packing, was selected for separation of TEL and BND. Different solvent systems were tried and optimized in combinations as mobile phase. TEL (40 μg/ml) and BND (4 μg/ml) in buffer, pH 4.0: Methanol (50:50) was developed as it was showing good peak shapes and a significant amount of resolution. The mobile phase was flowed at 1.0 ml/min with detection of both the analytes at 210 nm using photodiode array detector.Result: Development of method was done, and validation was accomplished using specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. The method was found linear from 20 to 60 μg/ml and 2–6 μg/ml for TEL and BND individually. The percentage recoveries of TEL 100.46% and BND100.08% were, respectively.Conclusion: This stability indicating RP-HPLC methods were developed by degradation of sample and compared with standard. The percentage relative standard deviation was also <2 % showing high degree of precision of the proposed method. The proposed method can be used for routine analysis of benidipine HCl and TEL in combined dosage form and quality control in bulk manufacturing.

scholarly journals Development of Validated RP-HPLC Method for Estimation of Empagliflozin and Metformin in Combined Formulation

2021 ◽  
pp. 1-7
Author(s):  
Vichare Vijaya ◽  
Kandekar Ujjwala ◽  
Dhaware Pallavi ◽  
V. P. Choudhari
Keyword(s):  
Detection Limit ◽  
Stationary Phase ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Phase Detection ◽  
Quantitation Limit ◽  
Rp Hplc ◽  
Accuracy And Precision

Aim: The aim of the present study include development of validated RP-HPLC method for estimation of Empagliflozin and Metformin in combined dosage form by using LC-MS compatible volatile mobile phase. Methodology: Appropriate separation of drugs was achieved using C18 column as a stationary phase and Acetonitrile: Water (50: 50, v/v) at a flow rate 1mL/min as mobile phase. Detection was done at 230 nm. Results: The Rt of Metformin and Empagliflozin was found to be 2.20 ± 0.02 min and 3.64 ± 0.02 min respectively. When the marketed formulation was analyzed by the developed method, the % drug contents were found to be 98.57 ± 1.28 and 99.86 ± 1.02 %w /w for Empagliflozin and Metformin, respectively. The method was found to be linear in a range of 11.25 – 56.25 μg/mL for Empagliflozin and 85 – 425 μg/mL for Metformin. Detection limit and quantitation limit were found to be 0.30 and 0.92 μg/mL for Empagliflozin and 1.12 and 3.36 μg/mL for Metformin, respectively. The accuracy and precision results were found to be near 100 % w/w for both the drugs. The method was also found to be robust and specific. Conclusion: The developed RP-HPLC method was found to be linear, sensitive, accurate,     precise, specific and robust for the analysis of Empagliflozin and Metformin in combined dosage form.

scholarly journals A new stability-indicating RP-HPLC method for the determination of dicyclomine hydrochloride and dimethicone combination in tablet dosage forms

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
J. Saroja ◽  
Anantha Lakshmi P.V. ◽  
Y. Rammohan ◽  
D. Divya Reddy
Keyword(s):  
Liquid Chromatography ◽  
Dosage Forms ◽  
Flow Speed ◽  
Hplc Method ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Rp Hplc ◽  
Tablet Formulations ◽  
Tablet Dosage

Abstract Background We describe a “stability-indicating liquid chromatography” technique for the estimation of dimethicone (DEC) and dicyclomine hydrochloride (DEH) in the established tablet formulations. Individual quantification of DEH and DEC was reported. But simultaneous quantification of DEH and DEC was lacking. DEH and DEC were analysed on an “XTerra C18 column (250 mm × 4.6 mm, 5 μm)” with the mobile phase solvent run isocratically with 0.1M K2HPO4-acetonitrile (55:45, v/v) on a flow speed of 1.0 mL/min. Results The chromatographic run period for the DEC and DEH assay was 6.0 min with retention times of 2.134 and 2.865 min, respectively. The method was validated for accuracy (99.453 to 100.417% and 99.703 to 100.303% recovery values for DEH and DEC, respectively), precision (RSV value 0.135% for DEC and 0.171% for DEH), linearity (5–15 μg/mL for DEH and 20–60 μg/mL for DEC), selectivity (no hinderance from excipients) and specificity (no hinderance from degradants) recovery. Conclusion The developed stability-indicating liquid chromatography process was well applied to established tablet formulations.

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