scholarly journals Quality risk assessment and DoE – Practiced validated stability-indicating chromatographic method for quantification of Rivaroxaban in bulk and tablet dosage form

2022 ◽  
Keyword(s):  
Method Development ◽  
Quadratic Model ◽  
Forced Degradation ◽  
Linear Calibration ◽  
Pareto Chart ◽  
Degradation Study ◽  
Saturation Time ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Hptlc Method

Abstract A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.

Development and Validation of Stability Indicating HPTLC Method for Estimation of Salmeterol Xinafoate

2019 ◽  
Vol 10 (01) ◽  
Author(s):  
Damle M ◽  
Choudhari S
Keyword(s):  
Quantitative Estimation ◽  
Degradation Study ◽  
Stability Indicating ◽  
Salmeterol Xinafoate ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Aluminium Sheets ◽  
Development And Validation ◽  
Chloroform Methanol ◽  
Hptlc Method

A simple, rapid validated stability indicating HPTLC method for estimation of Salmeterol xinafoate was successfully developed. This method is based on HPTLC separation followed by UV detection at 252 nm. The separation was carried out on Merck TLC aluminium sheets precoated with silica gel 60F254 using Chloroform: Methanol: Ammonia (7:3:0.5 v/v/v) as a mobile phase and scanning was done by using TLC Scanner III. Salmeterol xinafoate gave well defined and sharp peak at Rf 0.52 ± 0.05 at 252 nm. Calibration curve was linear in range 1000-3000 ng/band for Salmeterol xinafoate. Stress degradation study includes hydrolysis under different pH, oxidation, thermal and photolytic conditions. The suitability of this HPTLC method for quantitative estimation of Salmeterol xinafoate was proved by validation in accordance with requirements of ICH guidelines Q2A (R1).

scholarly journals Stress Degradation Assessment of Lamotrigine Using a Validated Stability-Indicating HPTLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Karim Michail ◽  
Hoda M. Daabees ◽  
Youssef Beltagy ◽  
Magdi Abdel-Khalek ◽  
Mona M. Khamis
Keyword(s):  
Linear Regression Analysis ◽  
Stress Factors ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stress Degradation ◽  
Forced Degradation Studies ◽  
Neutral Media ◽  
Tablet Formulations ◽  
Hptlc Method

In this work, a sensitive and stability-indicating HPTLC method for the determination of lamotrigine is presented. According to the International Conference on Harmonization guidelines Q1A, lamotrigine was exposed to a variety of stress conditions; these include heating in acidic, basic and neutral media. Its stability towards oxidative stress, humidity, high temperature and direct sunlight was also examined. Separation of the drug from its forced degradation impurities was achieved using TLC silica gel plates and a mobile phase composed of ethyl acetate: methanol: ammonia. The linear regression analysis of the data obtained for the correlation plots showed good linearity over the concentration range of 10–300 ng/spot. The forced degradation studies showed that lamotrigine is susceptible to degradation under acidic, basic, neutral and oxidative conditions, among which alkaline-induced hydrolysis had the highest degradative potential. Alternatively, the drug was stable under heat, humidity, and daylight stress factors. In order to assess the purity and stability of the drug in tablet formulations, the developed method was applied to the analysis of commercial tablets in brand and generic products. The obtained results showed that the degradation of the drug has not occurred in the marketed formulations that were analyzed by the described methodology.

scholarly journals RP-HPLC-PDA Method Development, Validation and Stability Studies of the Novel Antineoplastic Drug Combination - Decitabine and Cedazuridine

2020 ◽  
pp. 10-16
Author(s):  
B. Mohammed Ishaq ◽  
L. Siva Sanker Reddy ◽  
S. Venu ◽  
M. Sreenivasulu ◽  
K. Vanitha Prakash
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Isosbestic Point ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Linear Calibration ◽  
Rp Hplc ◽  
Stress Degradation ◽  
Bulk Drug

Aim: The aim of our present work was to develop and validate a reverse phase high-performance liquid chromatography (RP-HPLC) method for the simultanious determination of Decitabine (DEC) and Cedazuridine (CED). Methodology: The developed method was further applied to observe the degradation of analytes under the influence of different forced degradation conditions. Analytes were resolved on C18, 250 x 4.6 mm, particle size 5 µm Xterra column, using a mobile phase combination of 0.1% Ortho Phospharic Acid buffer pH 6.5: Methanol (40:60v/v) with flow rate of 1mL/min and injection volume of 10 µL. Quantification was carried out with PDA detector at an isosbestic point of 220 nm with a linear calibration curve in the concentration range of 35-175 μg/mL for DEC and 100-500 μg/mL for CED. Results: Validation of the developed method was performed as per ICH guidelines viz., linearity, accuracy, precision, and robustness. The limits of detection (LOD) and the limits of quantification (LOQ) for CED were found to be 2.69 µg/mL and 8.15 µg/mL respectively. LOD and LOQ for DEC 1.55 µg/mL and 4.68 µg/mL respectively. Moreover, validated method was applied to study the degradation profile of analytes under various stress degradation conditions. Conclusion: The proposed method was found to be sensitive, specific and was successfully applied for the simultaneous estimation of Decitabine (DEC) and Cedazuridine (CED) in bulk drug, and tablets.

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

scholarly journals AN INNOVATIVE METHOD DEVELOPMENT AND FORCED DEGRADATION STUDIES FOR SIMULTANEOUS ESTIMATION OF SOFOSBUVIR AND LEDIPASVIR BY RP HPLC

2018 ◽  
pp. 34-41
Author(s):  
B. Anjaneyulu Reddy ◽  
Md. Irshad Alam ◽  
Nazia Khanam ◽  
P. R. Adhakrishnanand
Keyword(s):  
High Performance ◽  
Method Development ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Effective Stability

Objective: To develop an innovative, rapid, simple, cost effective, stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for simultaneous estimation of ledipasvir (LP) and sofosbuvir (SB) in combination pill dosage form. Methods: The method was developed using C8 column, 250 mm x 4.6 mm, 5mm using mobile section comprising of 0.1% (v/v) orthophosphoric acid buffer at pH 2.2 and acetonitrile in the ratio of 45:55 that was pumped through the column at a flow rate of 0.8 ml/min. Temperature was maintained at 30 °C, the effluents were monitored at 260 nm with the help of usage of PDA detector. Results: The retention time of LP and SB were found to be 2.246 min and 3.502 min. The approach was found to be linear with the variety of 9-36 µg/ml and 40-240 μg/ml for LP and SB respectively, the assay of estimated compounds were found to be 99.65% and 99.73% w/v for LP and SB respectively. Conclusion: The pressured samples changed into analyzed and this proposed a technique turned into determined to be particular and stability indicating as no interfering peaks of decay compound and excipients were observed. Hence, the approach was easy and economical that may be efficiently applied for simultaneous estimation of both LP and SB in bulk and combination tablet system.

scholarly journals Determination of Rosuvastatin in the Presence of Its Degradation Products by a Stability-Indicating LC Method

2005 ◽  
Vol 88 (4) ◽  
pp. 1142-1147 ◽  
Author(s):  
Tushar N Mehta ◽  
Atul K Patel ◽  
Gopal M Kulkarni ◽  
Gunta Suubbaiah
Keyword(s):  
Degradation Products ◽  
Stability Study ◽  
Tablet Formulation ◽  
Assay Method ◽  
Forced Degradation ◽  
Degradation Study ◽  
Stability Indicating ◽  
Degraded Samples ◽  
Accelerated Stability

Abstract A forced degradation study was successfully applied for the development of a stability-indicating assay method for determination of rosuvastatin Ca in the presence of its degradation products. The method was developed and optimized by analyzing the forcefully degraded samples. Degradation of the drug was done at various pH values. Moreover, the drug was degraded under oxidative, photolytic, and thermal stress conditions. Mass balance between assay values of degraded samples and generated impurities was found to be satisfactory. The proposed method was able to resolve all of the possible degradation products formed during the stress study. The developed method was successfully applied for an accelerated stability study of the tablet formulation. The major impurities generated during the accelerated stability study of the tablet formulation were matches with those of the forced degradation study. The developed method was validated for determination of rosuvastatin Ca, and the method was found to be equally applicable to study the impurities formed during routine and forced degradation of rosuvastatin Ca.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR ESTIMATION OF SWERTIAMARIN IN BULK AND DOSAGE FORM

2017 ◽  
Vol 9 (6) ◽  
pp. 80
Author(s):  
H. Padh ◽  
S. Parmar ◽  
B. Patel
Keyword(s):  
High Performance ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Bulk Drug ◽  
Development And Validation ◽  
Layer Chromatography ◽  
Herbal Formulations ◽  
Hptlc Method ◽  
Ich Guideline

Objective: In the present study a novel stability-indicating high-performance thin-layer chromatography (HPTLC) method for quantitative determination of Swertiamarin (SW) in bulk drug and formulation has been developed and validated as per ICH guideline Q2 (R1) for global acceptance of standardized herbal formulations.Methods: HPTLC method is developed and validated using solvent ethyl acetate: ethanol: chloroform (3:2.5:4.5 v/v/v) (Rf of SW 0.65±0.04) in the absorbance mode at 243 nm. Various forced degradation conditions were used to check degradation of drug.Results: The method showed a good linear relationship (r2 = 0.9990) in the concentration range 200-700 ng per spot. It was found to be linear, accurate, precise and specific.Conclusion: It can be applied for quality control as well as for stability testing of different dosage forms containing swertiamarin. The developed method is validated as per ICH guideline Q2(R1) for global acceptance of standardized herbal formulations.

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