scholarly journals Method Development and Validation of Degradation Studies of Favipiravir by RP-HPLC

2021 ◽  
pp. 220-228
Author(s):  
. Shyamala ◽  
Dongamanti Ashok
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Analytical Standards ◽  
Theoretical Plates

RP HPLC method was developed by this study estimation of favipiravir. This method is developed by Shimadzu LC -2010 HT by using a C18 (250 X 4.6 X mm X 5µ) column in solvents Water(OPA)+ACN  (60:40)v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate of 1ml/min was pumped and sample wavelength was detected at 324 nm by ultraviolet -visible spectrophotometer. The Rt was found 4.453 min. The number of theoretical plates and tailing factor for favipiravir was observed 82651(NLT 2000) and 1.265 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, LOD, LOQ and robustness. LOD and LOQ values were calculated from regression of favipiravir 1.26 and 3.83 µg/ml.The regression equation of validated method for favipiravir is Y=253.5x+1881.In a wide range of 4 to 20 (µg/ml) the linearity was observed. Degradation methods were also performed.

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 Method Development and Validation of RP-HPLC Method for the Estimation of Ormeloxifene

2017 ◽  
Vol 2 (03) ◽  
pp. 78-82
Author(s):  
Anusha Shivaraj ◽  
Shireesha Battula
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Isocratic Mode ◽  
Ich Guideline

A new simple, specific, accurate, precise RP-HPLC method has been developed for the estimation of Ormeloxifene. The chromatographic separation for Ormeloxifene was achieved with mobile phase containing methanol :ACN(70:30 v/v), agilent C18 column (4.6 x150 mm) 5 μ at room temperature and UV detection at 274nm.The compounds were eluted in the isocratic mode at a flow rate of 1ml/min. The retention time of Ormeloxifene was found to be 2.497min. The method was validated according to ICH guideline for linearity, specificity, precision, accuracy, LOD, LOQ and robustness in accordance with ICH guidelines.

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

INDIAN DRUGS ◽  
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.

Method Development and Validation of Degradation Studies of Lenalidomide by RP-HPLC

2021 ◽  
pp. 4281-4286
Author(s):  
Punna Venkateshwarlu ◽  
Mehul M. Patel
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
System Suitability ◽  
Wide Range

A simple, accurate, RP HPLC method was developed by this study determination of lenalidomide. This method is developed by Shimadzu LC -2010 HT by using C18 (250 X 4.6 X mm X 5µ) column in solvents Phosphate buffer: Acetonitrile (55:45) v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate 1ml/min was pumped and sample wavelength was detected at 242nm by ultraviolet -visible spectrophotometer. The retention time was found 2.5 min. The number of theoretical plates and tailing factor for lenalidomide was observed 16199.817 (NLT 2000) and 1.128 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, system suitability and robustness. LOD and LOQ values obtained from regression of lenalidomide 0.058 and 0.174µg/ml. The regression equation of validated method for lenalidomide is Y=5223x+183075. In wide range of 25 to 150 (µg/ml) the linearity was observed. The method was validated and a recovery study indicates accuracy of this method. The Retention time less compared to established methods. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lenalidomide in bulk drug and in its pharmaceutical dosage forms.

scholarly journals Novel Stress Indicating RP-HPLC Method Development and Validation for the Simultaneous Estimation of Ertugliflozin and Sitagliptin in Bulk and its Formulation

2018 ◽  
Vol 34 (5) ◽  
pp. 2554-2561
Author(s):  
D. China Babu ◽  
C. Madhusudhana Chetty ◽  
S. K. Mastanamma
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

A selective, sensitive RP-HPLC method was developed for the simultaneous estimation of the Ertugliflozin (ETR) and Sitagliptin (SGT) in bulk and its dosage form. The separation and determination was carried on water’s C18 column capacitate (250X4.6 mm, 5 µm particle size), retention times of Ertugliflozin and Sitagliptin were found to be 2.39 and 4.60 min respectively. The wavelength was fixed at 215nm with PDA detection. The mobile phase was consisted mixture of 0.5 mM potassium dihydrogen ortho phosphate buffer: Methanol in the ratio of 55:45 v/v, pH 5.3 was adjusted with HCl and flow of mobile phase was maintained 1mL/min. The calibration curve was linear and regression co-efficient (R2) value found to be 0.999 and concentration ranging from 37.5-112.5 and 250-750 µg/mL for Ertugliflozin & Sitagliptin respectively. The quantization limit and detection limit of the method were found 0.1 & 0.3 µg/ml and 0.4&1µg/ml for Ertugliflozin & Sitagliptin.

scholarly journals Method Development and Validation of Fludrocortisone Acetate Tablets by Reverse Phase HPLC Method

2020 ◽  
Vol 11 (4) ◽  
pp. 6826-6833
Author(s):  
Vijey Aanandhi M ◽  
Elancheziyan K ◽  
Yamini R ◽  
Prakash Chand T ◽  
Aysha Jadeera K A ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Hplc Technique ◽  
Fludrocortisone Acetate ◽  
Development And Validation

The purpose or intent of this current study was to establish a fast and sensitive HPLC technique for the perseverance of Fludrocortisone acetate and utilizing best frequently used HPLC technique. This method had been validated as per the ICH requirements  to assure that the method consistently meets the predetermined specifications and quality attributes.Utilizing filtered and degassed pH 3.0 Phosphate buffer and Acetonitrile in the ratio 90:10 as a Mobile phase-A and pH 3.0 Phosphate buffer and Acetonitrile in the ratio 65:35 as a Mobile phase-B the established RP-HPLC technique was done. The separation was achieved by using Waters, X-Bridge Shield RP18, (150 X 4.6-mm), 3.5-µm column. Run time and Flow rate was set 45minutes and 1.2mL/min. Injection volume 100µL and wavelength was set 240nm.The correlation coefficient square for fludrocortisones acetate and Fludrocortisone Impurity was found to be 0.9991 and 0.99997. The SD and %RSD for Fludrocortisone Impurity was found to be 0.02 and 1.48 represents method precision. Following validated parameters lies within the limit. Hence, the developed method was precise, simple, fast and accurate.

scholarly journals A New Quantitative Analytical Method Development and Validation for the Analysis of Boceprevir in Bulk and Marketed Formulation

2018 ◽  
Vol 10 (03) ◽  
Author(s):  
Bhetanabotla Chandramowli ◽  
B.M Syam Kumar ◽  
D.V. R. N. Bhikshapathi ◽  
Bigala B Rajkamal
Keyword(s):  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Capsule Formulation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and accurate RP-HPLC technique was developed and the developed method was validated for the regular analysis of Boceprevir. Chromatographic analysis was performed by selecting X-Terra ODS ( C18) column (4.6 mm i.d. × 250 mm, 5μ), Acetonitrile : Phosphate buffer pH -3 ( 90 : 10% v/v) as mobile phase, 1.0 ml/min as flow rate and 20μl injection volume. The LC chromatographic peak was eluted at 3.6 min at 235 nm as UV detection wavelength. The developed method was validated as per the ICH guidelines and the Validation parameters were specificity, accuracy, linearity, precision, LOD and LOQ. Linear relationship for Boceprevir established in the concentration range of 50 to 150μg/mL. Accuracy in terms of percentage recovery found in the range between 98 to 101%. LOD and LOQ values were found to be 2.3 and 7.123μg/mL respectively. The results of the method established that the new RP-HPLC method is convenient and simple in regular analysis of Boceprevir in bulk and capsule formulation.

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

INDIAN DRUGS ◽  
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

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 Method Development and Validation of Polmacoxib in Capsule Dosage Form by RP-HPLC

2021 ◽  
Vol 11 (4-S) ◽  
pp. 59-63
Author(s):  
Anjali Chaudhary ◽  
Meenakshi Dhaiya ◽  
Shaily Tyagi ◽  
Swati Mittal
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Intended Use

A simple and sensitive RP-HPLC method developed for estimation of Polmacoxib in bulk by using a high performance liquid chromatography with PDA detector using Phenomenex luna C18 column (250mmx4.6mm), 5 µm; mobile phase comprises of Water : ACN as (1:1) at the flow rate 1.0 ml/min and the wavelength of detection  238 nm and eluted at 8.12 minutes. The proposed method is validated for specificity, Linearity, Precision, accuracy, ruggedness, and Robustness. All the parameters were found within the acceptable limits. RP-HPLC method was a simple, reliable economic and acceptable and it confirmed that method is suitable for the intended use for routine quality control and assay of drugs. This method is successfully applied for the determination of commercial dosage form capsule preparation. This method is validated as per ICH (International conference on harmonization) Guidelines. Keywords: Polmacoxib, RP-HPLC, ICH, PDA Detector, Precision

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