Analytical Method Development and Validation of Stability Indicating assay method of analysis for Dolutegravir/Lamivudine/Tenofovir Disoproxil Fumarate tablets using High Performance Liquid Chromatography

2021 ◽  
pp. 2434-2439
Author(s):  
Saravanan. R ◽  
Somanathan. T ◽  
Gavaskar D ◽  
Tamilvanan M
Keyword(s):  
Development Strategy ◽  
Tenofovir Disoproxil Fumarate ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Equilibration Time ◽  
Elution Time ◽  
Detailed Method ◽  
The Stability

A novel, economic, simple, precise and time-efficient reverse-phase high performance liquid chromatographic (RPHPLC) method has been established for the simultaneous assay determination of Dolutegravir, Lamivudine and Tenofovir Disoproxil fumarate in tablet formulation. This research paper presents the detailed method development strategy and the outcome of validation challenges. The RPHPLC method was developed using a 150 x 4.6mm, 5µm C18 column, with a gradient mode using 0.1% (v/v) trifluoroacetic acid buffer and methanol, the detection was performed at 260nm. The method was validated for specificity, precision, linearity, accuracy, robustness and can be used in quality control during manufacture and for assessment of the stability samples of Dolutegravir/Lamivudine/Tenofovir Disoproxil fumarate tablets. Total elution time was about 5 min and equilibration time of about 2 min which allows analysis of more than 100 samples per day. The method reported in this study is compatible to mass spectrometry and is thus extremely useful for stability studies.

STABILITY INDICATING RP - HPLC METHOD DEVELOPMENT FOR THE SIMULTANEOUS ESTIMATION OF LAMIVUDINE, TENOFOVIR DISOPROXIL FUMARATE AND EFAVIRENZ IN BULK AND PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (11) ◽  
pp. 57-63
Author(s):  
V. Suryadevara ◽  
◽  
R. L Sasidhar ◽  
B. Venkateswara Rao ◽  
T. N. V. Ganesh Kumar ◽  
...  
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
High Performance ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Hplc Method Development ◽  
Liquid Chromatographic

A simple, accurate reverse phase high performance liquid chromatographic method has been developed for the simultaneous estimation of lamivudine, tenofovir disoproxil fumarate and efavirenz in bulk and pharmaceutical formulations. The analytical method development was carried on Agilent make HPLC instrument using RP - C18 column. The mobile phase employed for the estimation is phosphate Buffer pH 4.0 :acetonitrile adjusted to pH 4.0 with glacial acetic acid which was pumped at a flow rate of 1.0 mL min-1 in the ratio of 42:58 v/v. the eluents were monitored at 260 nm. Linearity was obtained in the concentration range of 20-100 μg/mL of lamivudine, tenofovir disoproxil fumarate and 100-500 μg/mL efavirenz. Degradation studies shows that all the three drugs were not degraded under acidic, alkaline, thermal and photolytic conditions.The method was statistically validated and RSD was found to be within limits. Due to its simplicity, rapidness, high precision and accuracy, the proposed HPLC method can be applied for determining lamivudine, tenofovir disoproxil fumarate and efavirenz in bulk and in pharmaceutical dosage form.

scholarly journals Assay method development and validation for butamben drug substance by using high performance liquid chromatographic technique

2020 ◽  
Vol 11 (1) ◽  
pp. 981-984
Author(s):  
Sachin D. Zade ◽  
Padma S. There ◽  
Sunanda S. Aswale ◽  
Shashikant R. Aswale
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Drug Substance ◽  
Assay Method ◽  
Forced Degradation ◽  
Chromatographic Technique ◽  
Relative Standard

Stability indicating assay methodology was developed with UV detection for the simultaneous quantification of Butamben drug substance by HPLC. The separation between degradation impurities and the peak due to Butamben was achieved by using Universal C 18, (100 x 4.6) mm, 5.0-micron column. Mobile Phase was made up of Water, Methanol and Orthrophosphoric acid by mixing 350:650:1 ml, respectively. Isocratic method was used by using flow rate of 1.0 ml/min, UV at 250 nm and column oven temperature at 50°C. Relative standard deviation for standard preparation under system precision was achieved within acceptance criteria. Relative standard deviation for retention time was achieved 0.11%, which shows reproducibility during replicate injections. After the successful development of this method, chemically forced degradation was performed by external acid, alkali and peroxide treatment. Not any degradation peak was interfering with any impurity. This newly developed innovative method is found suitable for the Assay analysis of Butamben API.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR EVALUATING THE STABILITY PARAMETERS FOR THE SIMULTANEOUS ESTIMATION OF CLOPIDOGREL BISULPHATE AND OMEPRAZOLE USING RP-HPLC

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (01) ◽  
pp. 60-67
Author(s):  
J. B Nagavi ◽  
◽  
B. M. Gurupadayya
Keyword(s):  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Stress Conditions ◽  
Simultaneous Estimation ◽  
Stability Parameters ◽  
Ich Guidelines ◽  
The Stability ◽  
Neutral Conditions

A simple, sensitive, accurate and specific stability-indicating high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of clopidogrel bisulphate and omeprazole in bulk. Extensive testing of clopidogrel bisulphate and omeprazole in different stress conditions were carried out as per the ICH guidelines Q1A (R2) Clopidogrel bisulphate and omeprazole was exposed to various stress conditions like oxidation, hydrolysis, photolysis and neutral decomposition. Clopidogrel bisulphate, which was found to degrade considerably in acidic and photo conditions, was found to be stable in alkaline and neutral conditions, whereas omeprazole was found to be degrading in alkaline, oxidative and photo conditions, but stable in acidic and neutral condition. Apart from the formation of minor degraded products under accelerated conditions, the drugs were reasonably stable in solid state. A good linear relationship over the concentration range of 50-500μg/mL was shown. Validation of the method was carried out as per the ICH guidelines. The method developed was found to be specific, selective, precise and accurate. Clopidogrel bisulphate showed degradation in 5M hydrochloric acid at 80oC, in 3% hydrogen peroxide for 5min the drug showed around 35% of degradation, when exposed to sunlight for 15 min, forming around 25-30% of degradation products. Omeprazole showed 15-18% degradation in alkaline and photo condition.Statistical analysis shows that the method is reproducible and selective for the estimation of clopidogrel bisulphate and omeprazole in dosage form.

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF MIDODRINE HYDROCHLORIDE IN BULK AND TABLETS

2016 ◽  
Vol 8 (9) ◽  
pp. 283 ◽  
Author(s):  
Hemant K. Jain ◽  
Kishor N. Gujar ◽  
Varsha A. Randhe
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Forced Degradation ◽  
Hplc Assay ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
The Stability

<p><strong>Objective: </strong>To develop an accurate, simple, sensitive and precise stability indicating reverse phase-high performance liquid chromatographic (RP-HPLC) assay method for estimation of Midodrine hydrochloride (MD) in bulk and tablets.</p><p><strong>Methods: </strong>The chromatographic separation was performed on enable C<sub>18</sub>, (250 mm X 4.6 mm, 5 μm) column. The mobile phase consists of triethylamine buffer 0.02%, pH-3: acetonitrile (38:62 v/v) was delivered at a flow rate of 0.6 ml/min and UV detection at 289 nm. The method was validated with forced degradation studies as per ICH guidelines.</p><p><strong>Results: </strong>The retention time of the drug was found to be 3.56 min. The developed method was found to be linear in a concentration range of 19.98-99.9μg/ml of the drug (r<sup>2</sup>= 0.9998). The low value of % RSD indicates reproducibility of the method. The low value of LOD and LOQ suggests the sensitivity of the method. The results of forced degradation studies indicated that the drug was stable in acidic condition and degraded in basic, oxidative and hydrolytic conditions.</p><strong>Conclusion: </strong>The present study represents first stability-indicating HPLC assay method that deals with the estimation of midodrine hydrochloride. It can be concluded from the results that the developed method is simple, rapid, accurate, specific, sensitive and precise. Thus, this method can be used for routine analysis of midodrine hydrochloride formulation and to check the stability of bulk samples.<p> </p>

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

Bioanalytical method development and validation of simultaneous analysis of telmisartan and hydrochlorthiazide in human plasma using LC-MS/MS

2016 ◽  
Vol 5 (03) ◽  
pp. 4862 ◽  
Author(s):  
Mathew George* ◽  
Lincy Joseph ◽  
Arpit Kumar Jain ◽  
Anju V.
Keyword(s):  
Human Plasma ◽  
Retention Time ◽  
High Performance ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Internal Standard ◽  
Assay Method ◽  
Buffer System ◽  
Internal Standards

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.

Method Development and Validation of Propofol by Reverse Phase HPLC and its Estimation in Commercial Formulation

2021 ◽  
pp. 3139-3142
Author(s):  
Kuntal Mukherjee ◽  
S. T. Narenderan ◽  
B. Babu ◽  
Survi Mishra ◽  
S. N. Meyyanathan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase Hplc ◽  
Liquid Chromatographic Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, sensitive and rapid high performance liquid chromatographic method has been developed for the determination of Propofol. The main focus of the method was to determine Propofol in solution form as well as in marketed formulation. Chromatographic separation was achieved on Inertsil ODS-3V column (250mm x 4.6mm; 5µm) with a mobile phase consisting of methanol: water (85:15), with a flow rate of 1.0ml/min (UV detection at 270nm). Linearity was observed over the concentration range of 10-110µg/ml with a regression equation y=88048x + 44524 and having a regression value (R2) of 0.999. The LOD and LOQ values found to be 10ng and 100ng, respectively. No changes found in ruggedness and robustness studies. The percentage of recovery was found to be 95.25% to 101.81%. Validation studies revealed that the method was specific, accurate, precise, reliable, robust, reproducible and suitable for the quantitative analysis in its pharmaceutical formulations.

scholarly journals Validation of developed method by RP-HPLC for estimation of Prasugrelin human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 13 (1) ◽  
pp. 65-75
Author(s):  
Kumar S. Ashutosh ◽  
Debnath Manidipa ◽  
Rao J.V.L.N. Seshagiri ◽  
Sankar D. Gowri
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
The Stability

This paper is concern with a reverse phase high performance liquid chromatography (RP-HPLC) bio-analytical method development and validation for Prasugrel in human plasma using photo diode array detector (PDA detector). The HPLC separation was carried out in an isocratic mode on an X-Terra C18 column (4.6 x 150 mm; 5 μm) with a mobile phase consisting of potassium dihydrogen phosphate [pH 3.0] and acetonitrile in the ratio of 30:70 v/v at a flow rate of 1.0 mL/min. The run time was maintained for 5 mins and the detection was monitored at 210 nm. The percentage recovery was found 99.61-100.06 in human plasma. This reveals that the method is quite accurate. The linearity was found 15-40 μg/mL in human plasma. The inter-day and intra-day precision in plasma was found within the limits. The lower limit of quantification (LLOQ) obtained by the proposed method was 0.05 μg/mL. The percentage relative standard deviation (%RSD) obtained for the drug spiked in plasma for stability studies were less than 2 %.Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 65-75

scholarly journals Method Development and Validation of Metoprolol and Felodipine by using RP-HPLC in Bulk and Pharmaceutical Dosage Form

2020 ◽  
Vol 11 (4) ◽  
pp. 8047-8053
Author(s):  
Potturi Ramadevi ◽  
Kantipudi Rambabu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Preparations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Concentration Limit ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

The main objective of this research is to develop and validate a simple, specific, precise, sensitive, cost effective and rapid Reversed-Phase High-Performance Liquid Chromatographic (RP-HPLC) method for simultaneous quantification of Felodipine and Metoprolol in bulk and pharmaceutical dosage forms. The separation of the analytes were carried out on a X-bridge phenyl column with a moving phase composed of 0.1 % Tri ethyl amine: acetonitrile (30:70 v/v) delivered at a stream of 1.0 ml/min, and separation has been observed by UV detector, at a detection wavelength of 235 nm. This method was proven to be linear over a concentration limit of 10-150 µg/ml for Metoprolol, 2-30 µg/ml for Felodipine with correlation coefficient of 0.999. The retention time of Metoprolol and Felodipine were 2.936, 4.535 minutes respectively. To separate Metoprolol and Felodipine peaks a run time of 8 min. was used. The validation results were in good agreement with acceptable limits. RSD values which are less than 2.0 % indicating the accuracy and precision of this method. Hence it was evident that the proposed method was said to be a suitable one for the regular analysis and quality control of pharmaceutical preparations which contain these active drugs either individually or in combination.

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