scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF DOLUTEGRAVIR AND RILPIVIRINE IN BULK AND PHARMACEUTICAL DOSAGE FORM AND ITS APPLICATION TO RAT PLASMA

2019 ◽  
pp. 267-271
Author(s):  
VEERASWAMI B ◽  
NAVEEN VMK
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Study Results ◽  
Relative Standard

Objective: The present paper describes a simple, accurate, and precise reversed-phase high-performance liquid chromatography (HPLC) method for rapid and simultaneous quantification of dolutegravir (DTG) and rilpivirine (RPV) in bulk and pharmaceutical dosage form and rat plasma. Methods: The chromatographic separation was achieved on Phenomenex C18 (150x4.6mm, 5μm). Mobile phase contained a mixture of 0.1% Ortho phosphoric acid and acetonitrile in the rato of 60:40 v/v, flow rate 1.0ml/min and ultraviolet detection at 262nm. Results: The retention time of DTG and RPV was 4.35 min and 7.73 min, respectively. The proposed method shows a good linearity in the concentration range of 10–150 μg/ml for DTG and 5–75 μg/ml for RPV under optimized conditions. Precision and recovery study results are in between 98 and 102%. In the entire robustness conditions, percentage relative standard deviation is <2.0%. Degradation has minimum effect in stress condition and solutions are stable up to 24 h. DTG and RPV drugs are release 98% at 2 h in rat body. Conclusion: This method is validated for different analytical performance parameters like linearity. Precision, accuracy, limit of detection, limit of quantification, robustness, and pharmacokinetic study were determined according to the International Conference of Harmonization (ICH) Q2B guidelines. All the parameters of validation were found in the acceptance range of ICH guidelines. The same method is also applied for plasma samples study in bioanalytical work.

scholarly journals STABILITY INDICATING VALIDATED HPLC METHOD FOR THE DETERMINATION OF ZANUBRUTINIB IN BULK AND PHARMACEUTICAL DOSAGE FORM

2020 ◽  
pp. 159-162
Author(s):  
M. VIJAYA KUMARI ◽  
CH. BALASEKHAR REDDY
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Acceptable Limit ◽  
Relative Standard

Objective: An accurate, rapid economical and straight forward, reliable assay technique was evolved and showed for the evaluation of zanubrutinib using reversed-phase high-performance liquid chromatography. Methods: In the proposed method, efficient chromatographic separation was achieved applying acetonitrile and 0.1% orthophosphoric acid (50:50 v/v) as a mobile phase with a flow of 1 ml/min and the wavelength was observed at 220 nm. Chromatography was administered isocratically at ambient temperature and run time was approximately 6 min and the retention time (Rt) was observed as 4.358 min. Results: The method was justified as per ICH guidelines. System suitability parameters were studied by injecting the quality six fold and results were well under acceptance criteria. Linearity study was administered between 10% and 150% levels, regression coefficient value was observed as 0.999. Limit of detection and limit of quantification were observed as 0.02 μg/ml and 0.2 μg/ml, respectively. Precision was found to be 0.74 for repeatability and 0.68 for intermediate precision. Recovery of the drug was found to be 98–102%, indicates that the recovery is in the acceptable limit. Validation results were found to be satisfactory and the method applicable for bulk and formulation analysis. Hence, it was evident that the proposed method was said to be suitable for regular analysis and quality control of pharmaceutical preparations. Conclusion: The validation results were in good agreement with the acceptable limit. Relative standard deviation values which are <2.0% indicating the accuracy and precision of this method. Assay of retail formulation was administered and found to be 100.24% was present using the above method. Stress conditions of degradation in acidic, alkaline, peroxide, and thermal were studied. This developed method showed reliable, precise, accurate results under optimized conditions.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

METHOD DEVELOPMENT AND VALIDATION OF OLANZAPINE IN PURE AND PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (02) ◽  
pp. 20-26
Author(s):  
V.S Mastiholimath ◽  
◽  
P.M. Dandagi ◽  
A.P. Gadad ◽  
N.V Murali Krishna ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Hplc Method ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Ammonium Hydrogen

A simple and reliable reverse phase high-performance liquid chromatography method was developed and validated for Olanzapine in pure and pharmaceutical dosage form. The method was developed on BDS Hypersil C18, (150 mm x 4.6 mm, 3μm) with a mobile phase of 0.01M tetra butyl ammonium hydrogen sulphate : methanol (80:20 v/v). The effluent was monitored by SPD-M20A, prominence UV-VIS detector at 234 nm. Calibration curve was linear over the concentration range of 10 –60μg/ml For interday and intraday precision % relative standard deviation values were found to be 0.18% and 0.24% respectively. Recovery of olanzapine was found to be in the range of 99.93 -100.00%. The limit of detection (LOD) and quantitation (LOQ) were 0.39275 and 1.1901μg/ml, respectively. The retention time and run time was very short; hence it is cost effective, making it more economical and rapid. Also this method can be used for the analysis of large number of samples.

DEVELOPMENT AND VALIDATION OF NOVEL STABILITY INDICATING RP-HPLC METHOD FOR QUANTIFICATION OF TOLVAPTAN IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (03) ◽  
pp. 62-68
Author(s):  
Khaleel Noorbasha ◽  
S. K. Abdul Rahaman
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Reversed Phase ◽  
Hplc Method ◽  
Working Standard ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Bulk Drug

Specific stability-indicating reversed-phase high performance liquid chromatography (HPLC) method has been developed and validated for the quantification of tolvaptan in bulk drug and pharmaceutical dosage form. The optimized conditions for the developed HPLC method are; Inertil ODS-3V column (150 x 4.6 mm, 5.0 mm) maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 40:60%v/v on isocratic mode at flow rate of 1.0 mL/min and detection wavelength 254 nm. The retention time of tolvaptan was found to be 2.59 min with linearity in the concentration range from 37.5 – 225.0 µg/mL, respectively. The mean percentage recovery of tolvaptan was found to be 98.30 – 101.13 %, respectively. The percent relative standard values were less than 2.0 at all the levels and indicates a satisfactory accuracy and precision. The robustness of the method found to meet the acceptance criteria. The stress study against qualified working standard of Tolvaptan, indicated that the developed HPLC method was stability- indicating, conducted as per ICH requirements. The developed method can be handy in the quality control of bulk and pharmaceutical dosage forms.

scholarly journals A STUDY OF METHOD DEVELOPMENT, VALIDATION AND FORCED DEGRADATION FOR SIMULTANEOUS QUANTIFICATION OF CABOZANTINIB AND NIVOLUMAB IN BULK AND PHARMACEUTICAL DOSAGE FORM BY RP-HPLC

2019 ◽  
pp. 102-106
Author(s):  
GOPINATH K ◽  
YANADIRAO M ◽  
PAVANI Y ◽  
SUBBA RAO M
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Simultaneous Quantification ◽  
Study Results ◽  
Relative Standard

Objective: The present paper describes a simple, accurate, and precise reversed-phase high-performance liquid chromatography (HPLC) method for rapid and simultaneous quantification of cabozantinib (CZT) and nivolumab (NVM) in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on Luna C18 (150 mm×4.6 mm, 3.5 μm). Mobile phase contained a mixture of 0.1% orthophosphoric acid and acetonitrile in the ratio of 50:50 v/v, flow rate 1.0 ml/min, and ultraviolet detection at 222 nm. Results: The proposed method shows a good linearity in the concentration range of 20–300 μg/ml for CZT and 5–75 μg/ml for NVM under optimized conditions. Precision and recovery study results are in between 98 and 102%. In the entire robustness conditions, percentage relative standard deviation is <2.0%. Degradation has minimum effect in stress condition and solutions are stable up to 24 h. Conclusion: This method is validated for different parameters such as precision, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ), ruggedness, robustness, and forced degradation study were determined according to the International Conference of Harmonization (ICH) Q2B guidelines. All the parameters of validation were found to be within the acceptance range of ICH guidelines. Since there is no HPLC method reported in the literature for the estimation of CZT and NVM in pharmaceutical dosage forms, there is a need to develop quantitative methods under different conditions to achieve improvement in sensitivity, selectivity, etc. The author declares the interest to develop a validation and forced degradation for simultaneous quantification of CZT and NVM.

scholarly journals Development and Validation of rp-HPLC Method of Cabozantinib in Active Pharmaceutical Ingredient and Pharmaceutical Dosage form

2021 ◽  
pp. 81-90
Author(s):  
Amruta A. Chaudhary ◽  
Ashwini V. Shelke ◽  
Anil G. Jadhav
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc

A specific, accurate rp-HPLC (reversed-phase high performance liquid chromatographic) method was developed for the quantification of Cabozantinib. The effective separation was achieved through reversed-phased C18 column 4.6 x 250 mm, 5µm using a mobile phase Methanol: phosphate buffer (ph. 3.00) with orthophosphoric acid (OPA) (55:45 % v/v). The flow rate of the mobile phase was found to be 0.8 mL/min. The detection was carried at a wavelength of 244 nm. The retention time of Cabozantinib was found to be 3.702 min. The correlation coefficient was found to be 0.9999. The developed method was accurately validated in the terms of accuracy, linearity range, precision, system suitability, robustness, limit of detection and limit of quantification. The details presented in this test will be useful for industrial application for determining Cabozantinib in active pharmaceutical ingredient and pharmaceutical dosage form.

scholarly journals New RP-HPLC Method Development and Validation for Dorzolamide in Ophthalmic Dosage Form

2018 ◽  
Vol 2018 ◽  
pp. 1-5
Author(s):  
Boovizhikannan Thangabalan ◽  
Getu Kahsay ◽  
Tadele Eticha
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Hplc Method Development ◽  
Liquid Chromatographic

A reversed phase liquid chromatographic method with UV detection at 254 nm for dorzolamide assay in ophthalmic solutions was developed and validated. Chromatographic separation was achieved on a Zorbax SB C18 (250 mm × 4.6 mm, 5 µm) column kept at 30°C with an isocratic mixture of mobile phase (phosphate buffer, pH 2.5, and acetonitrile, 90 : 10 v/v) at a flow rate of 0.8 mL/min. The method was validated for its specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness based on ICH guidelines. The validation studies revealed satisfactory results. The proposed method has been applied for the quantification of dorzolamide in commercial samples. The developed method is fast, simple, specific, accurate, and sensitive, hence can be applied for routine quality control analysis of dorzolamide in pharmaceutical dosage form.

scholarly journals Development and Validation of Bioanalytical HPLC Method For Estimation of Telmisartan In Rat Plasma: Application To Pharmacokinetic Studies

2013 ◽  
Vol 11 (2) ◽  
pp. 121-127 ◽  
Author(s):  
Jaydeep M Patel ◽  
Anjali P Dhingani ◽  
Kevin C Garala ◽  
Mihir K Raval ◽  
Navin R Sheth
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmacokinetic Parameters ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Liquid Chromatographic

A simple, specific, sensitive and rapid reversed phase high performance liquid chromatographic (HPLC) method has been developed and validated for the determination of telmisartan in small volumes of rat plasma. Biological sample preparation involving simple extraction with organic solvent, followed by dilution with mobile phase was adopted to eliminate any chromatographic solvent effects. The method was proven to be linear over a plasma concentration range of 10 to 1000 ng/mL with a mean correlation coefficient of 0.9942. The limit of detection and the limit of quantification of the newly developed method were determined to be 1 ng/mL and 10 ng/mL, respectively. The method was successfully applied to assess pharmacokinetic parameters of telmisartan in Wister rats following a single oral dose (1.8 mg/kg, b.w.). The developed method was established as a rapid analytical tool in a pharmacokinetic study as it required short retention time, high precision, sensitivity and small volumes of plasma for analysis. DOI: http://dx.doi.org/10.3329/dujps.v11i2.14562 Dhaka Univ. J. Pharm. Sci. 11(2): 121-127, 2012 (December)

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

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