scholarly journals Stability Indicating RP-HPLC Method Development for Related Substances of Anti-histamine Promethazine hydrochloride and its Validation study

2020 ◽  
Vol 36 (05) ◽  
pp. 889-896
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopal Krishnan ◽  
Mannathusamy Mannathusamy ◽  
Raja Rajan Govindasamy
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Potassium Hydroxide Solution ◽  
Hplc Method ◽  
Concentration Limit ◽  
Forced Degradation ◽  
Control Analysis ◽  
Related Substances ◽  
Rp Hplc ◽  
Promethazine Hydrochloride

A smooth, specific, precise, and accurate high-performance reverse phase (RP-HPLC) method for determining related substances in antihistamine Promethazine Hydrochloride (PMZ∙HCI) has been recorded. The RP-HPLC system is developed and tested in compliance with recommendations Q2(R1) of the International Council for Harmonization (ICH). Column 5m and reverse step with linear gradient elution is accomplished in Symmetry Shield RP8 (4.6 mm x 150 mm). Mobile phase A is 3.4% in the 7.0 pH water, modified to dilute potassium hydroxide solution. In contrast, the 60:40 mixture of acetonitrile and methanol combination as mobile phase B. The handled phase with a continuous flow rate of 1.0 ml min-1 is provided by choosing the wavelength 254 nm using a PDA/UV detector. The temperature of the column oven and sampler is 25°C and 4°C, respectively. The injection amount chosen is 10.0 μL. The method is linear in the quantitation limit range (LOQ) to 150 percent concerning the specification impurity concentration limit. Both impurities and PMZ have a correlation coefficient of greater than 0.999. The LOQ for all known impurities and PMZs has a specification limit of between 10 to 30%. The relative response factor for all four known impurities is calculated. The unexplained peaks are very different; the effects obtained are similar to the original values. There are no significant changes improvements to the suitability parameters, such as tailing factor, Plates theoretical sheets, and % RSD in Robustness Studies. The forced degradation analysis of PMZ∙HCI was performed. This RP-HPLC is descriptive, accurate and precise. This further defines the parameters of linearity, consistency and robustness used for regular quality control analysis.

scholarly journals Stability Indicating RP-HPLC Method for Determination of Valsartan in Pure and Pharmaceutical Formulation

2010 ◽  
Vol 7 (1) ◽  
pp. 246-252 ◽  
Author(s):  
S. K. Patro ◽  
S. K. Kanungo ◽  
V. J. Patro ◽  
N. S. K. Choudhury
Keyword(s):  
Linear Response ◽  
Mobile Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Control Analysis ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quality Control Analysis ◽  
Rp Hplc

A simple, rapid and accurate and stability indicating RP-HPLC method was developed for the determination of valsartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 50-175 µg/mL using 0.01 M NH4H2PO4(pH 3.5) buffer: methanol [50:50] as the mobile phase with detection at 210 nm and a flow rate of 1 mL/min and retention time 11.041 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

scholarly journals VALIDATED GRADIENT STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF 11 RELATED SUBSTANCES IN THE COMBINED DOSAGE FORMS OF LAMIVUDINE AND TENOFOVIR DISOPEOXIL FUMARATE

2017 ◽  
Vol 9 (4) ◽  
pp. 61 ◽  
Author(s):  
C. Babu ◽  
N. Devanna ◽  
K. V.n. Suresh Reddy
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Related Substances ◽  
Drug Substances ◽  
Rp Hplc

Objective: Development of a stability-indicating reverse phase liquid chromatographic (RP-HPLC) method for the simultaneous quantification of 11 impurities in the combined dosage forms of lamivudine and tenofovir disoproxil fumarate drug substances.Methods: Efficient chromatographic separation of all analytes was achieved on a Waters X-terra RP18 column (150 x 4.6 mm, 3.5 mm) using mobile phase A (ammonium acetate buffer, pH adjusted to 5.0±0.05 with dilute orthophosphoric acid) and mobile phase B (mixture of methanol and ammonium acetate buffer in the ratio of 20:80) with the flow rate of 1.0 ml/min in gradient elution mode at 260 nm.Results: The method was validated in terms of the limit of detection, limit of quantification, linearity, accuracy, precision and robustness according to the international conference on harmonisation (ICH Q2R1). Regression analysis showed that the correlation coefficient (r2) is greater than 0.997 for individual active drug substances as well as their related substances. The method has proven very accurate (94.6 % to 108.2 % with % RSD not more than 4.9), highly precise (% RSD of the Intra-day and the inter-day study was not more than 8.9) and robust enough to deliver accurate results, when the chromatographic conditions were altered intentionally. Forced degradation studies were conducted in acidic, basic, thermal, photolytic, humid and peroxide stress conditions, where all the degradation peaks were monitored. Highest degradation of lamivudine was observed under oxidative stress condition and tenofovir was more susceptible to degradation under acidic and alkaline conditions.Conclusion: The present method is able to separate all the related compounds with each other and with the main drug substances with the resolution more than 2.0. The test solution was found to be stable in diluent up to 24 h. The mass balance of forced degradation of formulations, close to 99 %, made this method as a stability indicating method.

Method Development and Validation for Estimation of related Substances in Tilorone Dihydrochloride using RP¬-HPLC

2021 ◽  
pp. 3319-3324
Author(s):  
M. Zeba Baktiyar ◽  
B. Mohammed Ishaq ◽  
Siva Sanker Reddy L ◽  
Sreenivasulu M.
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Column Temperature ◽  
Related Substances ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and reproducible RP-HPLC method was developed for the estimation of related substances in tilorone dihydrochloride. Quantification was performed using a Zorbax SB-phenyl column (150 × 4.6mm, 5µ) with mobile phase A: 20mM potassium dihydro phosphate + 2ml of triethylamine, pH 2.30 and mobile phase B: acetonitrile, methanol and water 60: 20: 20% v/v. A gradient program was followed with a run time of 55 minutes at a flow rate of 1.0 ml/min. The column temperature was maintained at 40°C, the injection volume was 10 µl and the detection was performed at 269nm using a PDA detector. The retention time of Tilorone dihydrochloride was found to be 10.36 minutes. The proposed method has been validated according to the ICH guidelines for Linearity, Precision, Accuracy, LOD, and LOQ. The method was linear from 0.157 - 3.934μg/ml for standard, 0.153-3.820μg/ml and 0.166 - 4.140μg/ml for impurities, TLHC01 and TLHC02 respectively. The impurities TLHC01 and TLHC02 have been mapped in all stress conditions. The LOD and LOQ of TLHC01 were found at 1.757μg/ml and 5.857μg/ml and 1.919μg/ml and 6.396μg/ml respectively for TLHC02 respectively. Statistical analysis showed that the method was precision, reproducible, selective, specific and accurate for the analysis of Tilorone dihydrochloride and its impurities. The wide range of linearity, sensitivity, precision, short retention times and simple mobile phase have shown that the method is suitable for the routine quantification of mass impurities of tilorone hydrochloride and its dosage pharmaceutical forms with high precision and accuracy.

scholarly journals Analytical Method Development and Validation for the Estimation of Sugammadex

2020 ◽  
Vol 10 (1) ◽  
pp. 52-59
Author(s):  
Rajashree Mashru ◽  
Hemangi Parekh ◽  
Parin Chokshi
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Distilled Water ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Isocratic Mode ◽  
Ich Guideline

A simple, precise, accurate, specific RP-HPLC method developed for sugammadex in bulk and simulated mixture. Chromatographic separation is achieved by C18 column (250 x 4.6 mm, 5µ) in isocratic mode. The optimized mobile phase consists of acetonitrile and double distilled water in ratio of 20:80%v/v at a flow rate of 0.5mL/min and sugammadex was monitored at 210nm. Retention time of the drug was found to be 3.39min. The linearity obtained in range of 50 – 250 µg/mL.  %RSD mean for precision and %Recovery mean of the sugammadex were found to be 0.63 and 99.04% - 99.84% respectively. Stability indicating nature of RP-HPLC method was established by applying the degradation condition. The results indicate that developed RP-HPLC method would be suitable for estimation of drug in presence of degradant product. The above developed method was validated according to ICH guideline.  Keywords: Sugammadex, Assay, Simulated Mixture, Forced Degradation, Validation.

scholarly journals RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF MACITENTAN WITH ITS KNOWN AND UNKNOWN DEGRADATION IMPURITIES IN ITS TABLET DOSAGE FORM

2018 ◽  
Vol 10 (5) ◽  
pp. 81
Author(s):  
Jahanvee K. Trivedi ◽  
Chirag J. Patel ◽  
M. M. Patel
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Gradient Elution ◽  
Hplc Method ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Extensive Degradation ◽  
As Stress ◽  
Hplc Method Development ◽  
Tablet Dosage

Objective: To develop and validate macitentan with its known and unknown degradation impurities in its tablet dosage form.Methods: The RP-HPLC method for macitentan and its impurities was developed and three potential degradation impurities MCA-02, MCA-01 and degradation impurity and N-propyl derivative and N-N dimethyl derivative process impurities were separated. Chromatographic separation was achieved within 70 min on Inertsil C8 (250*4.6 mm, 5 µm) column, Using mobile phase A [Ammonium acetate (ph 4.5 adjusted with glacial acetic acid)] and mobile phase B acetonitrile in gradient elution. Other hplc parameter which was optimized flow rate 1.5 ml/min, detection wavelength 266 nm, column oven temperature 30 ° C and injection volume 20μl. macitentan was subjected to forced degradation also known as stress testing. It was validated as per ICH guidelines.Results: The drug showed extensive degradation in acidic and basic conditions, a slight degradation in oxidative condition. The developed method was statistically validated for linearity (0.45-2.25 ppm). The result of precision (%RSD<5), robustness, LOD(0.15 ppm) and LOQ(0.45 ppm) are well within limits.% Recovery at LOQ, 50%, 100% and 150% was found to be within limit 80-120 %.Conclusion: RP-HPLC method was successfully developed with satisfactory separation of macitentan and its impurities. The proposed method was found to be specific, accurate, precise and robust can be used for estimation of macitentan and its impurities and can be successfully employed in the routine analysis of macitentan.

scholarly journals RP-HPLC Method Development and Its Validation for Quantitative Determination of Rimonabant in Human Plasma

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Shravan Bankey ◽  
Ganesh Tapadiya ◽  
Jasvant Lamale ◽  
Deepti Jain ◽  
Shweta Saboo ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Hplc Method Development

A simple, accurate, and precise HPLC method was developed and validated for determination of rimonabant in human plasma. Following liquid-liquid extraction, chromatographic separation was accomplished using C18 column with mobile phase consisting of acetonitrile : water (90 : 10, v/v), drug was detected at 260 nm using UVdetector. The LOD and LOQ were 3.0 and 10.0 μg/L, respectively. The method is linear in the interval 50.0–1000.0 μg/L. The average extraction recovery of drug from plasma was found to be 92.2%. The percent CV of the method was found to be less than 10.8%, and accuracy was found between 94.5 and 106.7%. The assay may be applied to a pharmacokinetic and bioequivalence study of rimonabant.

scholarly journals AN INNOVATIVE METHOD DEVELOPMENT AND FORCED DEGRADATION STUDIES FOR SIMULTANEOUS ESTIMATION OF SOFOSBUVIR AND LEDIPASVIR BY RP HPLC

2018 ◽  
pp. 34-41
Author(s):  
B. Anjaneyulu Reddy ◽  
Md. Irshad Alam ◽  
Nazia Khanam ◽  
P. R. Adhakrishnanand
Keyword(s):  
High Performance ◽  
Method Development ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Effective Stability

Objective: To develop an innovative, rapid, simple, cost effective, stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for simultaneous estimation of ledipasvir (LP) and sofosbuvir (SB) in combination pill dosage form. Methods: The method was developed using C8 column, 250 mm x 4.6 mm, 5mm using mobile section comprising of 0.1% (v/v) orthophosphoric acid buffer at pH 2.2 and acetonitrile in the ratio of 45:55 that was pumped through the column at a flow rate of 0.8 ml/min. Temperature was maintained at 30 °C, the effluents were monitored at 260 nm with the help of usage of PDA detector. Results: The retention time of LP and SB were found to be 2.246 min and 3.502 min. The approach was found to be linear with the variety of 9-36 µg/ml and 40-240 μg/ml for LP and SB respectively, the assay of estimated compounds were found to be 99.65% and 99.73% w/v for LP and SB respectively. Conclusion: The pressured samples changed into analyzed and this proposed a technique turned into determined to be particular and stability indicating as no interfering peaks of decay compound and excipients were observed. Hence, the approach was easy and economical that may be efficiently applied for simultaneous estimation of both LP and SB in bulk and combination tablet system.

scholarly journals Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

2006 ◽  
Vol 71 (11) ◽  
pp. 1195-1205 ◽  
Author(s):  
Mira Zecevic ◽  
Biljana Jocic ◽  
Snezana Agatonovic-Kustrin ◽  
Ljiljana Zivanovic
Keyword(s):  
Mobile Phase ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Control Analysis ◽  
Internal Standard Method ◽  
Rp Hplc ◽  
Good Repeatability

Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax? tablets. The chromatography was performed at 20?C using a C18 XTerra ? (5 ?m, 150 x 4,6 mm) column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 %) - methanol (67.2:32.8 v/v), the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatability, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 - 1.00 mg/ml for eletriptan hydrobromide and from 0.10 - 1.50 ?g/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax? tables.

scholarly journals A Novel Stress Indicating RP-HPLC Method Development and Validation for the Simultaneous Estimation of Velpatasvir and Sofosbuvir in Bulk and Its Tablet Dosage Form

2019 ◽  
pp. 1-10 ◽  
Author(s):  
D. Chinababu
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Detection Range ◽  
Rp Hplc ◽  
Tablet Dosage

Aim: The objective of the study was simplest, accurate, precise and robust reversed phase high performance liquid chromatographic (RP-HPLC) method was developed for the estimation of Velpatasvir (VEL) and Sofosbuvir (SOF) in the bulk and its tablet dosage form. Study Design: The Quantitative and Qualitative estimation and designed forced degradation study of Velpatasvir & Sofosbuvir by RP-HPLC. Place and Duration of Study: The study was carried at Santhiram College of Pharmacy and time taken 4 months. Method: The method was attained by used Waters( 5µm, C18 250 x 4.6 mm) column with mobile phase consists of  0.5 mM disodium hydrogen phosphate buffer pH adjusted to 6.5, with Orthophosphoric acid and Methanol in the ratio of 78:22 v/v, a flow rate of 1.0 mL/min and ultraviolet detection at 285 nm. Results: The method was validated as per ICH guidelines with different parameters, the mean retention times of VEL and SOF were found to be 2.8 & 4.7 min respectively. The resolution between VEL and SOF was found to be 10.66. The Correlation coefficients for calibration curves within the detection range of 32.5 - 97.5 and 125 - 375 µg/mL were 0.999 for VEL and SOF respectively. The LOD and LOQ for VEL and SOF were found to be 0.0068-0.029 µg/mL and 0.104-0.342 µg/mL respectively. Conclusion: The results were indicated that the developed method was used for the routine analysis of VEL & SOF combined form in bulk and its commercial formulation. To the best of our knowledge, there was no method of RP-HPLC for the determination of VEL alone or in combination with SOF molecule.

Sign in / Sign up

Export Citation Format

Share Document