Development and Validation of RP-HPLC Method for the estimation of Sofosbuvir and Ledipasvir in combined dosage form

Nowadays scientists aim at developing generic and specific methods for drugs in combined pharmaceutical dosage forms. The main aim was to develop and carry out validation using precision and accuracy for Sofosbuvir and Ledipasvir by applying RP-HPLC method. The dosage form in fixed combination of Sofosbuvir-Ledipasvir helps in effective treatment of genotypes of chronic hepatitis C virus. This combination of Sofosbuvir-Ledipasvir was the first FDA approved direct acting antiviral to treat hepatitis C. Both the drugs were optimized using mobile phase as acetonitrile: 0.1% orthophosphoric acid (55:50v/v) with pH 3.0. The mobile phase was optimized at maximum wavelength of 283nm. The separation was achieved using C18 Cosmosil (4.6 x 250mm) column with a particle size of 5µ. The method was specific eluting retention times of 3.7 for Sofosbuvir and 6.0 for Ledipasvir. Intra and interday precision was carried and %RSD was found to be less than 2%. The results were found to be accurate with percentage recovery of 99.76% and 99.10% for Sofosbuvir and Ledipasvir respectively. Linearity was carried out in the concentration ranging from 40-200µg/mL and 9-45µg/mL for Sofosbuvir and Ledipasvir respectively. Both the drugs showed the regression coefficient of 0.999. Deliberate changes in flow rate, pH and wavelength were made and found that method was robust. The developed method was found to be accurate, simple, specific, robust and precise for the simultaneous estimation of Sofosbuvir and Ledipasvir in tablet dosage form.

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STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND AZILSARTAN MEDOXOMIL IN TABLET DOSAGE FORM

INDIAN DRUGS ◽

10.53879/id.53.06.10500 ◽

2016 ◽

Vol 53 (06) ◽

pp. 51-61

Author(s):

J. G Modi ◽

◽

J. K. Patel

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Hplc Method ◽

Simultaneous Estimation ◽

Good Resolution ◽

Amlodipine Besylate ◽

Stability Indicating ◽

Rp Hplc ◽

Tablet Dosage ◽

Azilsartan Medoxomil

A novel, simple, rapid, and highly selective stability indicating RP-HPLC method was developed and validated for simultaneous estimation of azilsartan medoxomil (AZL) and amlodipine besylate HCl (AMLO) in tablet dosage form having strength of 20 mg and 2.5 mg, respectively. The effective chromatographic separation was achieved on a Phenomenex luna ODS C18 (15 cm X 4.6 mm internal diameter, 3.5 μm Particle size) with a mobile phase composed of phosphate buffer (pH-2.5) adjusted with ortho phosphoric acid : acetonitrile in the ratio of 60:40 v/v. The mobile phase was pumped using an isocratic HPLC system at a flow rate of 0.7 mL/min with injection volume 20μl and quantification of the analytes was done at detection wavelength 254 nm. The retention times were found to be 5.918 min and 14.901 min for AMLO and AZL, respectively. The proposed HPLC method was validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, LOD, and LOQ as per ICH Q2 (R1) guideline. Calibration plots were linear over the concentration range of 75-125 µg/mL and 600-1000 µg/mL with correlation coefficients 0.9966 and 0.9948 for AMLO and AZL, respectively. Forced degradation studies were performed using hydrolysis, oxidation, photolytic, and thermal degradation conditions with good resolution between the degradants and analytes. Degradation products resulting from the stress studies did not interfere with the detection of AMLO and AZL, thus the proposed method is sensitive and stability-indicating. The validated HPLC method was successfully applied to the analysis of AMLO and AZL in tablet dosage form.

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RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF LINAGLIPTIN AND EMPAGLIFLOZIN

INDIAN DRUGS ◽

10.53879/id.56.05.11150 ◽

2019 ◽

Vol 56 (05) ◽

pp. 68-71

Author(s):

A Lakshmana Rao ◽

◽

T. Prasanthi ◽

E. L Anusha

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Method Development ◽

Hplc Method ◽

Simultaneous Estimation ◽

Rp Hplc ◽

Method Development And Validation ◽

Hplc Method Development ◽

Development And Validation ◽

Tablet Dosage

A simple, accurate and precise RP-HPLC method was developed for the simultaneous estimation of the linagliptin and empagliflozin in tablet dosage form. Chromatogram was run through Kromasil 250 x 4.6 mM, 5mM column, mobile phase containing 0.1% o-phosphoric acid buffer and acetonitrile in the ratio of 60:40%v/v was pumped through column at a flow rate of 1 mL/min. The optimized wavelength was 230 nm. Retention times of linagliptin and empagliflozin were found to be 2.759 min and 2.139 min. %RSD of the Linagliptin and Empagliflozin were found to be 0.5 and 0.6 respectively. Percentage assay was obtained as 99.91% and 100.15% for linagliptin and empagliflozin, respectively. LOD, LOQ values obtained for linagliptin and empagliflozin were 0.23 μg/ml and 0.44 μg/mL and 0.70 μg/mL and 1.34 μg/mL, respectively. Thus, the current study showed that the developed RP-HPLC method is sensitive and selective for the estimation of linagliptin and empagliflozin in combined dosage form.

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Analytical method validation for estimation of avanafil and dapoxetine hydrochloride tablet dosage form by HPTLC method

Pharmaceutical and Biological Evaluations ◽

10.26510/2394-0859.pbe.2017.26 ◽

2017 ◽

Vol 4 (3) ◽

pp. 171 ◽

Cited By ~ 3

Author(s):

Dhwani A. Shah ◽

Kunjal L. Vegad ◽

Ekta D. Patel ◽

Hitesh K. Prajapati ◽

Ronak N. Patel ◽

...

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Hplc Method ◽

Simultaneous Estimation ◽

Analytical Method Validation ◽

Rp Hplc ◽

Tablet Dosage ◽

Chloroform Methanol ◽

Hptlc Method ◽

Dapoxetine Hydrochloride

Objective: A simple, specific, accurate and precise RP-HPTLC method has been developed and validated for simultaneous estimation of Avanafil and Dapoxetine.Methods: The chromatographic separation was achieved on Aluminium plates precoated with Silica gel 60 F254 using chloroform: methanol: ethyl acetate: glacial acetic acid (5:2:3:0.2, v/v/v/v) as mobile phase detected at 279 nm.Results: The correlation coefficient for RP-HPLC method was found to be 0.9987 for Avanafil and 0.9991 Dapoxetine and the linearity range was found to be 1040-3640 ng*spot-1 for Avanafil and 80-280 ng*spot-1 for Dapoxetine.Conclusions: The developed method was successfully applied to marketed tablet dosage form and the results were found with higher confidence.

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ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ALISKIREN AND VALSARTAN IN BULK AND TABLET DOSAGE FORM BY RP-HPLC

INDIAN DRUGS ◽

10.53879/id.52.07.p0005 ◽

2015 ◽

Vol 52 (07) ◽

pp. 5-9

Author(s):

L Kalyani ◽

◽

A. L. Rao

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Method Development ◽

Hplc Method ◽

Simultaneous Estimation ◽

Rp Hplc ◽

Relative Standard ◽

Method Development And Validation ◽

Development And Validation ◽

Tablet Dosage

A simple, precise and accurate RP-HPLC method was developed and validated for the simultaneous estimation of aliskiren and valsartan in combined tablet dosage form. The chromatographic separation of the two drugs was achieved on Symmetry C8 column (250 x 4.6 mm, 5 μm). The mobile phase consisted of acetate buffer: acetonitrile (60:40 V/V) and pH was adjusted to 5.8 with glacial acetic acid was delivered at the flow rate of 1.4 mL/min and detection was performed at 220 nm. Separation was completed within 4 minutes. The calibration curves were linear with a correlation coefficient of 0.999 over the concentration range of 7.5 to 75 µg/mL of aliskiren and 8 to 80 µg/mL of valsartan. The relative standard deviation (RSD) was found

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Simultaneous estimation of telmisartan and atorvastatin calcium in API and tablet dosage form

Journal of Drug Delivery and Therapeutics ◽

10.22270/jddt.v9i1.2268 ◽

2019 ◽

Vol 9 (1) ◽

pp. 175-179 ◽

Cited By ~ 1

Author(s):

BANGARUTHALLI JAGIRAPU ◽

U Harini ◽

M Divya ◽

P Sushma

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Wave Length ◽

Hplc Method ◽

Simultaneous Estimation ◽

Atorvastatin Calcium ◽

Rp Hplc ◽

Ich Guidelines ◽

Tablet Dosage ◽

Column Flow Rate

A new method has been established for the simultaneous estimation of Telmisartan and Atorvastatin calcium by RP-HPLC method. The chromatographic conditions were successfully developed for the separation of Telmisartan and Atorvastatin calcium by using boston ODS C18 column, flow rate was 1.0ml/min, mobile Phase consists of methanol:Acetonitrile:buffer in ratio of 35:25:40. Detection wave length was 235nm.The instrument used was SHIMADZU HPLC auto sampler. The retention time of Atorvastatin calcium and Telmisartan was found to be 2.350 and 3.490 minutes respectively. The analytical method was validated according to ICH guidelines (ICH Q2b). The correlation coefficient (r2) was found to be 0.997 and 0.999 for Telmisartan and Atorvastatin calcium respectively. % mean recovery was found to be 100.943% and 100.576% for Telmisartan and Atorvastatin calcium respectively. %RSD for precision on replicate injection was 0.46 and 0.70 for Telmisartan and Atorvastatin calcium respectively. The validation study was found to be precise, robust, and repeatable. Keywords: Telmisartan, Atorvastatin calcium, ICH guidelines, Validation.

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Simultaneous Estimation of Gemcitabine Hydrochloride and Capecitabine Hydrochloride in Combined Tablet Dosage Form by RP-HPLC Method

E-Journal of Chemistry ◽

10.1155/2011/437157 ◽

2011 ◽

Vol 8 (3) ◽

pp. 1212-1217 ◽

Cited By ~ 2

Author(s):

V. Rajesh ◽

B. Anupama ◽

V. Jagathi ◽

P. Sai Praveen

Keyword(s):

Mobile Phase ◽

High Performance ◽

Dosage Form ◽

Limit Of Detection ◽

Hplc Method ◽

Simultaneous Estimation ◽

Gemcitabine Hydrochloride ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Tablet Dosage

A new reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous estimation of gemcitabine hydrochloride and capecitabine hydrochloride in combined tablet dosage form. An inertsil ODS-3 C-18 column having dimensions of 250×4.6 mm and particle size of 5 µm, with mobile phase containing a mixture of acetonitrile : water : triethyelamine in the ratio of (70 : 28 : 2v/v) was used. The pH of mobile phase was adjusted to 4.0 withortho-phosphoric acid. The flow rate was 1 mL/min and the column effluents were monitored at 260 nm. The retention time for gemcitabine hydrochloride and capecitabine hydrochloride was found to be 2.76 and 2.3 min respectively. The proposed method was validated in terms of linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The method was found to be linear in the range of 10-50 µg/mL and 4-24 µg/mL for gemcitabine hydrochloride and capecitabine hydrochloride, with regression coefficient r = 0.999 and r = 0.999, respectively.

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