Quantitative Stability Indicating Bio-analytical Method Development and Validation of Apalutamide - Apalutamide D3 By Using Ultra Performance Liquid Chromatography in Human Plasma

2020 ◽  
Vol 11 (4) ◽  
pp. 7740-7746
Author(s):  
China Babu D ◽  
Madhusudhana Chetty C ◽  
Mastanamma SK
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Internal Standard ◽  
Extraction Process ◽  
Ultra Performance Liquid Chromatography ◽  
Stability Indicating ◽  
Long Term Stability ◽  
Stability Indicating Method ◽  
The Stability ◽  
Liquid Chromatographic

A simple, convenient, specific, precise and highly conventional stability-indicating ultra-performance liquid chromatographic‑ diode array method was developed for the quantification of Apalutamide in human plasma. The Phenomenex Luna (100x4.6x5µ) column was used for apalutamide separation. The mobile phase was composed with 5 mM ammonium fumarate and acetonitrile in the ratio of 15:85 v/v, and buffer pH 3.5 was adjusted with glacial acetic acid and detected at 345 nm. The Apalutamide‑D3 used as internal standard and K2‑EDTA used as a coagulant. The liquid-liquid extraction process used for extraction of drug from human plasma with tert butyl methyl ether. The retention times of Apalutamide and Apalutamide D3 (ISTD) was 1.48 min & 1.97 min, respectively. The assay of the method was validated in human plasma in the concentration range from 307.26-200013.87 pg/ml with the accuracy and precision ranging from 3.86 to 4.87. Recovery studies were found to be 103.79%, 90.93% & 96.83% for HQC, MQC and LQC respectively. The stability of the drug was evaluated in human plasma with different conditions of the auto-sampler, freeze-thaw, bench top, short term and long term stability studies were performed. The method was proved as highly sensitive and selective for the quantification of Apalutamide and determined at the picogram level. There was no matrix effect observed and proved as a stability-indicating method. 

scholarly journals Stability indicating method development and validation for simultaneous estimation of atorvastatin calcium and celecoxib in bulk and niosomal formulation by RP-HPLC

2015 ◽  
Vol 51 (3) ◽  
pp. 653-661 ◽  
Author(s):  
Priyanka S. Jadhav ◽  
Priti M. Jamkar ◽  
Amelia M. Avachat
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Atorvastatin Calcium ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Bulk Drug ◽  
Development And Validation ◽  
Liquid Chromatographic

The present work describes development and validation of a specific, sensitive, precise and stability-indicating high-performance liquid chromatographic method of analysis of atorvastatin calcium and celecoxib, both as a bulk drug and in niosomal formulation. The analysis has been performed by using Cosmosil-C18 column (4.6 mm´250 mm, 5 m) at 25 °C using acetonitrile: ammonium acetate buffer pH 5.0: methanol (50:25:25 v/v/v) as mobile phase. The detection was carried out at 277nm with a flow rate of 1.0mL/min. The retention times of Atorvastatin calcium and Celecoxib were 6.195 and 3.989min, respectively. The method was validated according to ICH guidelines, for specificity, precision, linearity, accuracy and robustness. Atorvastatin calcium and Celecoxib were subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation was observed in oxidation and acid hydrolysis. The linearity for atorvastatin calcium and celecoxib were in the range of 100-500 µg/mL. The recovery study of atorvastatin and celecoxib were found to be in the range of 98.96 - 99.92% and 98.90-100%, respectively. The proposed method was validated and successfully applied to the estimation of Atorvastatin calcium and Celecoxib in combined in-house niosomal formulation.

scholarly journals Stability-indicating Reversed Phase-Ultra Performance Liquid Chromatography Method Development and Validation for Simultaneous Determination of Encorafenib and Binimetinib in Formulation

2020 ◽  
pp. 488-494
Author(s):  
Taduvai Venkata Raveendranath ◽  
Rajaiah Thangaraj Saravanakumar ◽  
Anjana Male
Keyword(s):  
Method Development ◽  
Detection System ◽  
Ultra Performance Liquid Chromatography ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Regression Equations ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Liquid Chromatography Method

A simple, accurate and precise stability indicating method was developed for the simultaneous estimation of the encorafenib (ECRB) and binimetinib (BMTB) in a dosage form by UPLC. Chromatographic elution was processed through a HSS C18 (100 x 2.1 mm, 1.8m) reverse phase column and the mobile phase composition of 0.01N KH2PO4 buffer (3.5 pH) and acetonitrile in the proportion of 55:45 was processed thru a column at a flow rate of 1.0 ml/min. Temperature of the column oven was kept at 30.0°C and the wavelength maximum of detection system was set to 294 nm. Retention times of ECRB and BMTB were found to be 0.767 min and 1.130 min respectively. Repeatability of the method was determined in the form of %RSD and findings were 0.3 and 0.6 for ECRB and BMTB respectively. The percentage recovery of the method was found to be 99.59% and 99.70% for ECRB and BMTB respectively. LOD, LOQ values obtained from regression equations of ECRB and BMTB were 0.51, 1.55mg/ml and 1.47, 4.44 mg/ml respectively. Regression equation of ECRB was y = 6684.x + 18102 and BMTB was y = 13118x + 2159. Two analytes were subjected for acid, peroxide, photolytic, alkali, neutral and thermal degradation studies and the results shown that the percentage of degradation was found between 0.76% and 6.88%. Retention times and total run time of two drugs were decreased and the developed method was simple and economical. So, the developed method can be adopted in industries as a regular quality control test for the quantification of ECRB and BMTB.

A Review article on Analytical Method Development for the combination of Azelnidipine and Telmisartan

2021 ◽  
pp. 227-234
Author(s):  
Nirma Chavda ◽  
Suresh Kumar
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Method Development ◽  
Ultra Performance Liquid Chromatography ◽  
Resonance Spectroscopy ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Layer Chromatography

The literature survey explains that there is not any stability indicating method reportedly for combination of Azelnidipine and Telmisartan till date. Validation and development of stability indicating analytical methods is possible as per ICH Guidelines. There are several of Spectroscopic methods such as Ultraviolet Spectroscopy, Mass spectroscopy, infrared spectroscopy, Nuclear magnetic resonance spectroscopy and Chromatographic methods such as High performance liquid chromatography, Thin layer Chromatography, High Performance thin layer chromatography, Gas chromatography and Ultra performance liquid chromatography etc. used for stability indicating method development and validation.

scholarly journals STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF PANOBINOSTAT LACTATEIN PHARMACEUTICAL DOSAGE FORMS BY UPLC

2018 ◽  
Vol 10 (11) ◽  
pp. 60
Author(s):  
Ashok Gorja ◽  
Sumanta Mondal
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method

Objective: The present study aimed to develop a stability indicating ultra-performance liquid chromatography (UPLC) method for the estimation of panobinostat lactate in pharmaceutical dosage form and validate the method in accordance with ICH guidelines.Methods: The optimized conditions for the developed UPLC method are acquity UPLC hibar C18 (100 mm × 2.1 mm, 1.8µ) column maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 50:50%v/v on isocratic mode at flow rate 0.3 ml/min. The sample was detected at 266 nm.Results: The retention time for panobinostat was found to be 1.6 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability. The method obeyed Beer’s law in the concentration range of 50µg/ml and 300µg/ml with correlation coefficient of 0.9998. Forced degradation studies were conducted by exposing the drug solution to various stress conditions such as acidic, basic, peroxide, neutral, photolytic and thermal conditions. The net degradation was found to be within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation ofpanobinostat can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals Stability indicating RP-UPLC method development and validation for the simultaneous determination of ertugliflozin and metformin in plasma

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 2417-2424
Author(s):  
Haritha G ◽  
Shanmugasundaram P
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Internal Standard ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Method Development And Validation ◽  
Resultant Solution ◽  
The Stability ◽  
Development And Validation

New stability-indicating RP-UPLC technique was developed for the quantification of ertugliflozin and metformin  in human plasma and validated as per the regulatory guidelines. Both the drug components and internal standard were spiked to blank plasma and subjected to liquid-liquid extraction with the mobile phase. The resultant solution was infused into Acquity BEH-C18 (1.7 μ, 100×2.1mm) non-polar column comprising NaH2PO4  buffer (pH-3.5), methanol and acetonitrile in the ratio of 50:10:40% v/v/v  as mobile phase. The detector response and flow of the mobile phase were monitored at 240nm and 0.5ml/min, respectively. The linearity plot was made in the concentration range of 0.1-3.0 µg/ml for metformin and 0.05-1.5 µg/ml for ertugliflozin with correlation coefficient value of more than 0.999. The developed method was subjected for bench-top, freeze and thaw, long-term and short-term stability studies and the drug components were stable over the respective conditions. The Lower limit of quantification (LLOQ) for ertugliflozin and metformin  were 0.05 and 0.1 µg/ml, respectively. The findings of precision and accuracy were present in between 2.6 to 4.2 %RSD and -2 to 3.99 %RE, respectively. The findings of the stability data were presented below. The %stability of ertugliflozin and metformin  were varying from 96% to 104% for ertugliflozin and 96% to 105% for metformin.

scholarly journals Method Development and Validation for Quantification of Sulfamethoxazole in Human plasma by UPLC-MS/MS

2021 ◽  
Vol 12 (1) ◽  
pp. 17-27
Author(s):  
Vijey Aanandhi M ◽  
Yamini R ◽  
Elancheziyan K ◽  
Prakash Chand T ◽  
Aysha Jadeera K A ◽  
...  
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Assay Method ◽  
Stability Parameters ◽  
Standard Curve ◽  
Carry Over ◽  
The Stability ◽  
Development And Validation

The main objective of the study aimed at developing and validating the advanced effective Liquid-Liquid Extraction  method for evaluating Sulfamethoxazole in Human plasma, by following the FDA guidelines using UPLC-MS/MS and Sulfamethoxazole D4 as Internal Standard. The analyte was eluted using Acetonitrile: 10mM Ammonium Formate pH 4.5 (60:40 v/v) flows through the column and flow-rate of 0.400mL/min. The injected volume set was 5µl. Chromatogram obtained with isocratic elution with efficient separation. Spiking concentrations were fixed for the Calibration Curve and Quality Control samples that produced the  linearity over the range of 320.635ng/ml to 22009.900ng/ml for the standard curve. The slope 0.0000535324  and corresponding intercept was plotted using the developed method. The method has been validated according to all established parameters of inter and intra precision and accuracy and showing recovery of 71.39% and 71.14% for SM and SMD4 respectively. Reinjection and Reproducibility and Auto Sampler Carry Over Test were met with the specifications. The validated method drew accuracy and meets specifications for the Big Batch, Hemolyzed and Dilution Integrity samples. This assay method was developed that proves all the stability parameters for the matrices as well as solutions used for the study and suitable for the bioequivalence study. The proposed method may also be applicable for the study of combined formulations.

scholarly journals Bioanalytical method development and validation for determination of metoprolol tartarate and hydrochlorothiazide using HPTLC in human plasma

2013 ◽  
Vol 49 (4) ◽  
pp. 845-851 ◽  
Author(s):  
Ambadas Ranganath Rote ◽  
Poonam Ramdas Sonavane
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Internal Standard ◽  
Analytical Technique ◽  
Method Development And Validation ◽  
Rf Values ◽  
The Stability ◽  
Development And Validation

A simple, sensitive, rapid and economic chromatographic method has been developed for determination of metoprolol tartarate and hydrochlorothiazide in human plasma using paracetamol as an internal standard. The analytical technique used for method development was high-performance thin-layer chromatography. HPTLC Camag with precoated silica gel Plate 60F254 (20 cm×10 cm) at 250 µm thicknesses (E. Merck, Darmstadt, Germany) was used as the stationary phase. The mobile phase used consisted of chloroform: methanol: ammonia (9:1:0.5v/v/v). Densitometric analysis was carried out at a wavelength of 239 nm. The rf values for hydrochlorothiazide, paracetamol and metoprolol tartarate were 0.13±0.04, 0.28±0.05, 0.48±0.04, respectively. Plasma samples were extracted by protein precipitation with methanol. Concentration ranges of 200, 400, 600, 800, 1000, 1200 ng/mL and 2000, 4000, 6000, 8000, 10000, 12000 ng/mL of hydrochlorothiazide and metoprolol tartarate, respectively, were used with plasma for the calibration curves. The percent recovery of metoprolol tartarate and hydrochlorothiazide was found to be 77.30 and 77.02 %, respectively. The stability of metoprolol tartarate and hydrochlorothiazide in plasma were confirmed during three freeze-thaw cycles (-20 ºC) on a bench for 24 hours and post-preparatively for 48 hours. The proposed method was validated statistically and proved suitable for determination of metoprolol tartarate and hydrochlorothiazide in human plasma.

scholarly journals Stability-Indicating Method Development and Validation for Simultaneous Estimation of Ombitasvir, Paritaprevir, and Ritonavir in Formulation by Ultra Performance Liquid Chromatography

2020 ◽  
pp. 457-463
Author(s):  
Samudrala Lakshmi Maneka ◽  
Rajaiah Thangaraj Saravanakumar ◽  
Anjana Male
Keyword(s):  
Method Development ◽  
Detection System ◽  
Research Work ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Formulation ◽  
Simultaneous Estimation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Alkaline Conditions ◽  
Development And Validation

Aim of the present research work was to develop a sensitive, precise and robust stability-indicating UPLC method for the simultaneous estimation of ombitasvir, paritaprevir and ritonavir in formulations. The chromatographic separation of mixture of ombitasvir, paritaprevir and ritonavir was attained in isocratic method utilizing a mobile phase of 0.01N Potassium dihydrogen orthophosphate (pH 5.3) and methanol in the proportion of 60:40%v/v utilizing a BEH C18 column which has dimensions of 100 x 3 mm, 1.7m particle size and the flow rate of 0.3 ml/min. The detection system was monitored at 252nm wavelength maximum with 0.2 ml injection volume. The retaining time for ombitasvir, paritaprevir and ritonavir was achieved at 1.765 min, 2.192 min, and 1.326 min respectively. Ombitasvir, paritaprevir and ritonavir and their combined drug formulation were exposed to thermal, acidic, oxidative, photolytic, and alkaline conditions. The present method was validated as per the guidelines given by the ICH for specificity, accuracy, sensitivity, linearity and precision. The developed method was highly sensitive, rapid, precise and accurate than the earlier reported methods. The total run time was decreased to 3.0 min; hence, the technique was more precise and economical. Stability studies directed for the suitability of the technique for degradation studies of ombitasvir, paritaprevir and ritonavir. The projected method can be utilized for routine analysis in quality control department in pharmaceutical trades.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION OF ITRACONAZOLE AND TERBINAFINE HCL IN BULK AND PHARMACEUTICAL TABLET DOSAGE FORM

2019 ◽  
pp. 51-55 ◽  
Author(s):  
DEVYANI M RODE ◽  
Dr. NUTAN RAO
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Pharmaceutical Tablet ◽  
The Stability ◽  
Tablet Dosage ◽  
Terbinafine Hcl

Objective: The objective of the present work was to develop and validate the stability-indicating method for the simultaneous estimation of itraconazole and terbinafine HCl in bulk and pharmaceutical tablet dosage form by reversed-phase high-performance liquid chromatography (HPLC). This combination of drugs is not reported for simultaneous HPLC analysis as of now. Methods: The analysis of the developed method was carried on Shimadzu LC Prominence-i 2030 model with Lab Solution software and the separation was done on Shim-pack C18 GIST (250 mm×50 mm, 5 μm) column with a flow rate of 1.2 ml/min and run time of 12 min. The injection volume was 10 μl and mobile phase consisted of acetonitrile and 0.1% triethylamine in the ratio of 90:10 and 225 nm was used as a detection wavelength. Results: The retention time was found to be 3.464 min and 8.705 min for itraconazole and terbinafine HCl, respectively. The calibration curve was found to be linear and r2 values were 0.9989 and 0.9995 for itraconazole and terbinafine HCl, respectively. Conclusion: The stability-indicating method was developed by subjecting itraconazole and terbinafine HCl marketed formulation to various stress conditions such as acidic, basic, oxidative, thermal, and water hydrolysis degradation conditions and the degraded product peaks were well resolved from sample peaks.

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