scholarly journals Validated stability indicating RP-HPLC method for the determination of dolutegravir and rilpivirine in bulk and pharmaceutical dosage forms

2021 ◽  
Vol 12 (3) ◽  
pp. 1961-1966
Author(s):  
Gopinath K ◽  
Padmavathi K. V. ◽  
Murali Krishna N ◽  
Subbarao M
Keyword(s):  
Drug Testing ◽  
Orthophosphoric Acid ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Acceptable Range ◽  
Ich Guidelines ◽  
Ethyl Amine

For simultaneous analysis of Dolutegravir and Rilpivirine utilizing RP-HPLC, an accurate, rapid, economical, quick and reliable assay technique was developed and tested. Successful chromatographic detachment using acetonitrile and 0.1 percent tri ethyl amine in the water of pH-2.5 adjusted with 0.1% orthophosphoric acid in 40:60 v/v as a movable phase with a flow of 1 ml/min and UV observation at 230 nm. Chromatography at ambient temperature was performed isocratically, and the run time was 10 min. By injecting the norm six times, device suitability parameters were studied and the findings were far below the acceptance criteria. The linearity analysis was performed at levels ranging from 10% to 150% and the R2 value was found to be 0.999. Precision has been found to be 0.8 for repeatability and 1.2 for intermediate precision. Assay of the commercialized formulation was performed by using the above method, and we get 100.01 percent was present. For routine analysis in drug testing, this chromatographic approach can be effectively implemented. By using the above technique, an assay of the marketed formulation was performed and found to be within the limit. Degradation studies were carried out on Dolutegravir and Rilpivirine, with a purity threshold greater than purity angle in all conditions and within the acceptable range. The above-mentioned technique was validated according to ICH guidelines. 

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

scholarly journals Simple, Accurate and Efficient High Performance Liquid Chromatographic Method for Determination of Vandetanib in Bulk and in Pharmaceutical Forms

2021 ◽  
pp. 153-160
Author(s):  
M. Murali ◽  
P. Venkateswara Rao
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, linear, precise and accurate isocratic RP-HPLC method was developed and validated for rapid assay of Vandetanib, an anticancer drug, in both bulk and tablet dosage form. Elution at a flow rate of 1ml/min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of acetonitrile, water and orthophosphoric acid in the ratio of 90:08:02 (v/v/v). Linearity was observed in concentration range of 50-200 ppm. The retention time for Vandetanib was 3.326 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Vandetanib in pharmaceutical dosage forms. Moreover the detection alone was also verified through LC-MS of the Vandetanib drug using ESI method which provides future scope for study of this drug using LC-MS method also.

Theophylline Determination in Pharmaceuticals Using a Novel High-performance Liquid Chromatographic Process

2021 ◽  
Vol 19 (7) ◽  
pp. 196-208
Author(s):  
H.N.K. AL-Salman ◽  
Ekhlas Qanber Jasim ◽  
Hussein H. Hussein
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
International Conference ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Chromatographic Process ◽  
Liquid Chromatographic

Objective: The current study aims to find a suitable, accurate, and faster RP-HPLC technique for the determination of theophylline, which could then be validated in accordance with the International Conference on Harmonization (ICH) guidelines. The Aim of this Study: The aim of this study was to develop an efficient, accurate, and faster RP-HPLC method for determining theophylline, which was then validated using the International Conference on Harmonization (ICH) guidelines. Methods: In the HPLC analysis, the Waters 2695 was used. The drug was isolated better using an Ion Pac zorbax 300-SCX Agilent Column, 5 m, 4.6 250 mm, with a liquid phase of Orthophosphoric acid (0.1 percent Orthophosphoric acid in HPLC acetonitrile and Methanol in the ratio of 50:50 v/v at a flow rate of 1ml/min, with discovery at 280 nm using a PDA detector. Results: Theophylline's preservation time was discovered to be 3.747 0.127 min. In the 5-25 mg/l range, the procedure was found to be linear, with a parallel coefficient (R2) of 0.9998. The LOD and LOQ of the system were determined to be (0.99 and 3) g/ml, respectively. The technique and system precisions were predicted using, and the outcomes were determined as percent RSD principles, which were noticed to be within the strict limitations. Theophylline recovery was detected to be in the 99-100 percent range, confirming the method's precision. Conclusion: Using basic ICH guidelines, the suggested RP-HPLC process was validated. The following methodology can be used successfully and easily for routine diagnostic analysis.

scholarly journals A Validated RP-HPLC Method for Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Formulations

2011 ◽  
Vol 8 (3) ◽  
pp. 1238-1245 ◽  
Author(s):  
G. Tulja Rani ◽  
D. Gowri Sankar ◽  
P. Kadgapathi ◽  
B. Satyanarayana
Keyword(s):  
Particle Size ◽  
Mobile Phase ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines

A simple, fast, precise, selective and accurate RP-HPLC method was developed and validated for the simultaneous determination of atenolol and indapamide from bulk and formulations. Chromatographic separation was achieved isocratically on a Waters C18 column (250×4.6 mm, 5 µ particle size) using a mobile phase, methanol and water (adjusted to pH 2.7 with 1% orthophosphoric acid) in the ratio of 80:20. The flow rate was 1 mL/min and effluent was detected at 230 nm. The retention time of atenolol and indapamide were 1.766 min and 3.407 min. respectively. Linearity was observed in the concentration range of 12.5-150 µg/mL for atenolol and 0.625-7.5 µg/mL for indapamide. Percent recoveries obtained for both the drugs were 99.74-100.06% and 98.65-99.98% respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method developed can be used for the routine analysis of atenolol and indapamide from their combined dosage form.

scholarly journals Validated stability indicating gradient RP-HPLC method for the estimation of antihypertensive drugs in bulk and pharmaceutical dosage forms

2012 ◽  
Vol 1 (11) ◽  
pp. 336-341 ◽  
Author(s):  
Napa Delhi Raj ◽  
Sockalingam Anbazhagan ◽  
Kunapareddy Anudeep Babu ◽  
Sunkara Narendra Babu ◽  
Chusena Narasimharaju Bhimanadhuni
Keyword(s):  
Antihypertensive Drugs ◽  
Degradation Products ◽  
Olmesartan Medoxomil ◽  
Pharmaceutical Journal ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines

A rapid and precise RP-HPLC method for determination of Olmesartan medoxomil and Hydrochlorothiazide in bulk and pharmaceutical dosage forms. Olmesartan medoxomil & Hydrochlorothiazide are found to be degraded together under different set of conditions as followed according to ICH guidelines and the degradants so formed along with olmesartan & hydrochlorothiazide are separated by using INERTSIL ODS C18 3V (150 x 4.6, 5µ) using mobile phase 1ml triethanolamine in one litre water and the pH was adjusted to 2.5 with orthophosphoric acid and acetonitrile using a gradient program with a flow rate of 1ml/min, throughout the gradient program with a detection wavelength of 225nm for both the compounds with a injection volume of 10µl. The method was validated for selectivity, linearity, accuracy, robustness, precision and specificity. The results were indicating the method was selective in analysis of both olmesartan medoxomil and hydrochlorothiazide in the presence of degradation products formed under various stress conditions.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12058 International Current Pharmaceutical Journal 2012, 1(11): 336-341

scholarly journals Validated Stability-Indicating RP-HPLC Method for the Determination of Norfloxacin in Pharmaceutical Dosage Form

2021 ◽  
Vol 10 (4) ◽  
Author(s):  
Sirajunisa Talath ◽  
Syeda Humaira
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

The objective of this work was to develop a simple, sensitive, accurate, precise and reproducible high performance liquid chromatography (HPLC) method for the determination of norfloxacin in pharmaceutical dosage forms. Shimadzo Prominance model L20 AD HPLC system equipped with SPD 20A UV-Vis detector was used for the analysis. The separation was done on RESTEX allure C18 column (3 μm, 15 cm × 4.6 mm), for an isocratic elution a mixture of methanol and water (60:40, v/v) mobile phase at a wavelength of 254 nm. The flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of norfloxacin was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness as per the ICH guidelines. The retention time of norfloxacin was 7.5 min. The linearity was established over the concentration ranges of 50-350 μg/mL with correlation coefficients ( r2) 0.999.  The percentage accuracy of norfloxacin ranged from 99.76 -101.66%. The relative standard deviation values for intra-day and inter-day precision was lower than 2.0% and the assay result was found to be 100.65 %. Norfloxacin was subjected to stress conditions such as neutral, acidic, alkaline, oxidation and photolysis degradations as per ICH guidelines. The degradation studies revealed that the drug was found to degrade maximum (1.67%) in alkaline degradation conditions and was highly resistant towards neutral, acidic, oxidative and photolytic degradation conditions. Keywords: Norfloxacin, Validation, Stability-indicating, stress degradation, ICH guidelines.  

scholarly journals Stability Indicating Validated HPLC Method for the Determination of Aceclofenac and Misoprostol in Bulk and Pharmaceutical Formulation

2020 ◽  
Vol 11 (4) ◽  
pp. 7848-7853
Author(s):  
Syed Rafi ◽  
Kantipudi Rambabu
Keyword(s):  
Room Temperature ◽  
Orthophosphoric Acid ◽  
Pharmaceutical Preparation ◽  
Hplc Method ◽  
Alkaline Peroxide ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Simultaneous Evaluation ◽  
Formulation Analysis

For the simultaneous evaluation of Aceclofenac and Misoprostol using RP-HPLC, an accurate, rapid, economical, and straightforward, reliable assay technique was developed and demonstrated. The proposed method achieved effective chromatographic separation by using an inertsil ODS column (150mmx4.6mm, 3.5), acetonitrile, and 0.1 percent orthophosphoric acid (OPA) (50:50 v/v) as a mobile phase with a flow rate of 1 ml/min and a wavelength of 227 nm. The retention time (Rt) of Aceclofenac was 3.189 minutes and Misoprostol was 6.966 minutes. Chromatography was performed isocratically at room temperature with a run time of around 10 minutes. The suitability parameters of the system were investigated by multiplying the quality six times, and the results were well within acceptable limits. The linearity analysis was conducted at 10 percent to 150 percent stages, with a regression coefficient of 0.999. Aceclofenac and Misoprostol had LOD and LOQ values of 0.063 ug/ml, 0.063 g/ml, and 0.208 ug/ml and 0.208 g/ml, respectively. The drug was recovered at a rate of 98-102 percent, which means that the recovery is within reasonable limits. The validation results were satisfactory, and the approach was found to be suitable for bulk and formulation analysis. As a result, it was obvious that the proposed approach was ideal for routine pharmaceutical preparation review and quality control. Validation results were very close to the appropriate maximum. RSD values of less than 2.0 percent indicate that this approach is accurate and precise. The above method was used to perform a retail formulation assay, which showed that 100.24 percent of the formulation was present. Degradation stress conditions in acidic, alkaline, peroxide, and thermal media were investigated. Under ideal conditions, the established method provided efficient, precise, and accurate results. According to ICH guidelines, the approach was justified.

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING HPLC METHOD FOR THE DETERMINATION OF NILOTINIB HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2016 ◽  
Vol 8 (9) ◽  
pp. 41
Author(s):  
Ramu Ivaturi ◽  
T. Manikya Sastry ◽  
S. Satyaveni
Keyword(s):  
Linear Regression Analysis ◽  
Analysis Data ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines

<p><strong>Objective</strong>:<strong> </strong>To develop a rapid, accurate, linear, sensitive and stability indicating RP-HPLC method for the determination of nilotinib in bulk and pharmaceutical dosage forms in the presence of its four related substances.</p><p><strong>Methods</strong>:<strong> </strong>The RP-HPLC method was developed for the chromatographic separation of nilotinib and its impurities by using waters Xterra RP-18 (150*4.6 mm, 3.5 µm) column with a mobile phase combination of 10 mM ammonium formate with pH-3.5 and acetonitrile in gradient mode. An injection volume of 20 µl. Flow rate was 1.0 ml/min and detection was carried a wavelength of 250 nm. The method was validated as per ICH guidelines.</p><p><strong>Results</strong>:<strong> </strong>The retention time for nilotinib and its four impurities were found to be 4.37, 7.40, 8.96, 10.21 and 10.87 min respectively. The linear regression analysis data for the calibration plots showed the good linear relationship in the concentration range of 0.04-3.0 ppm for the nilotinib impurities. The % recovery of nilotinib impurities was found to be 96.8-99.4% in the linearity range. The detection limit (LOD) values were about 0.014, 0.016, 0.005 and 0.03 ppm respectively and the quantification limit (LOQ) values were 0.042, 0.048, 0.014 and 0.09 ppm respectively. The % degradation at various stress conditions like acid, alkaline, oxidative, thermal and photolytic stress was found to be 8.92, 18.35,5.63, 0.88 and 3.89 respectively.</p><p><strong>Conclusion: </strong>The RP-HPLC method compatible with LC-MS was developed for the analysis of nilotinib and its four impurities. It was validated as per the ICH guidelines and found to be linear, robust, precise, accurate, sensitive, stability indicating and can be used for routine as well as stability analysis of capsule dosage forms as well as for drug substance.</p>

Development and Validation of Mebeverine Hydrochloride Assay by RP-HPLC Method

2018 ◽  
Vol 11 (5) ◽  
pp. 4239-4243
Author(s):  
Akbar Syed ◽  
Shaik Haroon Rasheed ◽  
Shaik Afroz ◽  
Syeda Wasfiya Noor ◽  
Syeda Saniya Fatima ◽  
...  
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Chromatographic Peak ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Mebeverine Hydrochloride ◽  
Development And Validation ◽  
Relationship Of

A validated method for the estimation of the mebeverine hydrochloride, an anti-spasmodic agent, was developed which was simple, precise, rapid and accurate. A clear separated chromatographic peak was achieved on Apollo C18 (4.6x250 mm), 5-μm column. Mobile phase used in this separation was the mixture of methanol and water in the ratio of 90:10% v/v with a flow rate of 0.9 μL/min at ambient temperature. The detection was achieved at a wavelength of 265 nm. At the retention time of 3.9 min and tailing factor of 1.09, chromatographic peak was observed. As per the guidelines of ICH, the method was developed and was validated with respect to accuracy, linearity, specificity, precision and robustness. Correlation co-efficient obtained shows a good linear relationship of more than 0.998 in the concentration range of 5 μg to 30 μg. Mean % recovery of 99.2% was seen and %RSD for repeatability and intermediate precision was less than 2%. Therefore, the developed method can be used for the quantitative determination of mebeverine hydrochloride successfully in pharmaceutical dosage forms.

scholarly journals Separation and Determination of Process Related Impurities in Palbociclib: A Rp-hplc Study

2021 ◽  
pp. 485-499
Author(s):  
D. Srikanth ◽  
S. Ganapaty ◽  
P. Manik Reddy ◽  
G. Sowjanya ◽  
K. Sunitha
Keyword(s):  
Signal To Noise Ratio ◽  
Hplc Method ◽  
Forced Degradation ◽  
Intermediate Precision ◽  
Related Impurities ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Quality Control Testing ◽  
Gradient Mode

Aims: A new gradient RP-HPLC method was developed for the separation and determination of process related impurities in Palbociclib. Methodology: The chromatographic separation was achieved on a Inert sustain swift (C18) column using a mobile phase comprising of perchloric acid and acetonitrile in a gradient mode at a flow rate of 1 mL/min. over a runtime of 50 minutes. All the eluants were monitored at 230 nm. The optimized method was validated as per ICH guidelines for various parameters. Results: The linearity of the method was proposed in the range of LOQ to 250 % for the drug and its impurities by subjecting the data obtained to statistical analysis using correlation coefficient model (r > 0.99). The method also gave acceptable recovery of all the four impurities at each level and was found to be accurate. The % RSD obtained in the method precision and intermediate precision were less than 2% depicting the precision of the method. The LOD and LOQ values were calculated based on the signal to noise ratio and are indicating the sensitivity of the method. The specificity of the method was checked in the presence of process related impurities and also degradants generated by exposing to a variety of forced degradation conditions. Conclusion: The proposed RP-HPLC method for the determination of process related impurities of Palbociclib could be routinely used in the quality control testing.

Sign in / Sign up

Export Citation Format

Share Document