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).

Development and validation of a new stability indicating RP-UFLC method for the estimation of Bosentan

2021 ◽  
pp. 4445-4451
Author(s):  
Kalyani Lingamaneni ◽  
Mukthinuthalapati Mathrusri Annapurna
Keyword(s):  
Blood Pressure ◽  
Pharmaceutical Formulations ◽  
Buffer Solution ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Pulmonary Arterial ◽  
Development And Validation ◽  
Alkaline Oxidation

A new stability-indicating RP-UFLC method has been developed for the estimation of Bosentan in pharmaceutical dosage forms and the method was validated. Bosentan is used to lower the high blood pressure in lungs (pulmonary arterial hypertension). Bosentan acts by blocking the actions of endothelin -1and thereby lowers the blood pressure. Mobile phase mixture consisting of sodium acetate (pH 5.0) buffer solution and acetonitrile (50: 50 v/v) with flow rate 0.7 mL/min were the optimized chromatographic conditions (Detection wavelength 254 nm) for the present study. Linearity was observed in the concentration range of 0.1–100 μg/mL (R2 = 0.9998) with regression equation y = 126698 x – 392.49. The LOQ was found to be 0.08964 µg/mL and the LOD was found to be 0.02913 µg/mL. Stress degradation studies such as acidic, alkaline, oxidation, photolysis and thermal degradations were performed by exposing Bosentan and finally the proposed method was validated as per ICH guidelines. The assay of Bosentan was conducted by applying the proposed method to the marketed formulations. The proposed method is simple, specific, precise, and accurate and can be applied for the estimation of pharmaceutical formulations.

scholarly journals Development and Validation of HPTLC Method for Studying Stress Degradation of Aspirin in Fulvic Acid Inclusion Complex

2020 ◽  
pp. 96-102
Author(s):  
Md. Khalid Anwer ◽  
Mohammed Muqtader Ahmed ◽  
Mohammad Javed Ansari ◽  
Mohammed F. Aldawsari ◽  
Mohd. Aamir Mirza
Keyword(s):  
Fulvic Acid ◽  
Inclusion Complexes ◽  
High Performance ◽  
Retention Factor ◽  
Molar Ratio ◽  
Forced Degradation ◽  
Ich Guidelines ◽  
Stress Degradation ◽  
Development And Validation ◽  
Hptlc Method

A new, precise high performance thin layer chromatographic (HPTLC) method for the analysis aspirin (ASP) in inclusion complexes with HPβCD and fulvic acid (FA) was developed and validated as per ICH guidelines. A precoated silica gel aluminium plate 60F-254 and a mixture of solvents, toluene: ethylacetate: formic acid (5:4:1 v/v) were used as stationary and mobile phase, respectively. This developed method was found to give an excellent defined sharp peak at a retention factor (RF) value of 0.52 ± 0.001. The LOQ and LOD values were found 35.29 and 123.54 ng / spot, respectively. The spray dried inclusion complexes of ASP/HPβCD and ASP/FA in the molar ratio 1:1, were subjected for forced degradation under stress conditions, and a significant reduction of ASP degradation were noted in complexed ASP as compared to ASP alone.

DEVELOPMENT AND VALIDATION OF HPTLC METHOD FOR QUANTITATIVE ESTIMATION OF PALIPERIDONE

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (09) ◽  
pp. 34-40
Author(s):  
A Shirode ◽  
◽  
C. Garade ◽  
V. Kadam
Keyword(s):  
Mobile Phase ◽  
Quantitative Estimation ◽  
Water Soluble ◽  
Uv Detector ◽  
Analytical Method Validation ◽  
Starting Position ◽  
Ich Guidelines ◽  
Sample Application ◽  
Development And Validation ◽  
Hptlc Method

A planar chromatography (HPTLC) method has been developed and validated for quantitative estimation of the atypical antipsychotic drug paliperidone, which is weakly basic and poorly water soluble. The Camag HPTLC system, operated by software winCATS (ver.1.4.1.8), was used. Sample application was facilitated by Linomat 5 applicator. After sample application, plates were subjected to ascending development in twin trough chamber of size 10 cm x10 cm, using about 10 mL of mobile phase. The optimized mobile phase was composed of ethyl acetate:chloroform:toulene:methanol (2.5:2.5:2.5:2.5 v/v/v/v). In post development, the plates were air dried and then scanned densitometrically using a UV detector at 278 nm in absorbance mode. In HPTLC densitogram, well defined peak was obtained for paliperidone with starting position at 0.27 Rf, max position at 0.31 Rf and end position at 0.34 Rf. The optimal Rf value for paliperidone was found to be 0.31. Performance characteristics of proposed and newly developed HPTLC method were statistically validated as per recommendations of ICH guidelines of analytical method validation. The HPTLC method was found to be linear across the range from 20 to 140 ng/band. The LOD and LOQ values were found to be 1.288 and 3.905ng/band, respectively. The method was found to be accurate, precise, robust and economical for the determination of paliperidone from bulk and its extended release tablet formulation.

scholarly journals STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF CLEVIDIPINE BUTYRATE IN SYNTHETIC MIXTURE

2018 ◽  
Vol 10 (6) ◽  
pp. 159
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Degradation Products ◽  
Standard Addition ◽  
Retention Factor ◽  
Economic Stability ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate stability indicating HPTLC method for determination of clevidipine butyrate in synthetic mixture.Methods: The present study deals with development and validation of stability indicating HPTLC method for estimation of clevidipine butryate. Chromatographic separation was performed on aluminum plate pre coated with Silica Gel 60 F254 using toluene: ethyl acetate (8:2) as mobile phase. TLC scanner was set at wavelength of 370 nm.Results: Retention factor Rf of clevidipine was found to be 0.49. The method was validated as per ICH guidelines. Calibration curve was in the range of 1000-6000ng/band. The correlation coefficient was found to be 0.999. The precision expressed by RSD was less than 2%. The accuracy of method was confirmed by recovery studies using standard addition method and recovery was found to be 99.03-99.57%. The drug was subjected to ICH prescribed hydrolytic, oxidative, photolytic and thermal stress conditions. Clevidipine and its degradation products were well resolved under experimental conditions. The method was validated according to ICH guidelines. The drug showed significant degradation in alkaline and acidic condition and slight degradation in oxidative condition. The drug was stable in thermal condition.Conclusion: A new, Simple, Accurate, Precise, Sensitive and economic stability indicating HPTLC method has been developed and validated for the determination of clevidipine and can be employed for stability indicating analysis.

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.

scholarly journals Development and Validation of Stability-Indicating HPTLC Method for Determination of Solifenacin Succinate as bulk Drug and in Tablet Dosage Form

2016 ◽  
Vol 8 (04) ◽  
Author(s):  
M.C. Damle ◽  
P. Rokade
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Retention Factor ◽  
Stability Indicating ◽  
Solifenacin Succinate ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Hptlc Method

A new simple, stability- indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for estimation of Solifenacin succinate in bulk and in tablet dosage form. The optimized mobile phase was Methanol: Water: Glacial acetic acid (9:1:0.1v/v/v) with UV detection at 216 nm. The retention factor for Solifenacin succinate was found to be 0.49 ± 0.03. The drug was subjected to stress conditions of hydrolysis under different pH conditions, oxidation, photolysis and thermal degradation as per ICH guidelines. Results were found to be linear in the concentration range of 2000-10000ng band-1.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

scholarly journals Development and Validation of Stability-Indicating HPLC Methods for the Estimation of Lomefloxacin and Balofloxacin Oxidation Process under ACVA, H2O2, or KMnO4 Treatment. Kinetic Evaluation and Identification of Degradation Products by Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5251
Author(s):  
Barbara Żuromska-Witek ◽  
Paweł Żmudzki ◽  
Marek Szlósarczyk ◽  
Anna Maślanka ◽  
Urszula Hubicka
Keyword(s):  
Room Temperature ◽  
Oxidation Process ◽  
Degradation Products ◽  
Isocratic Elution ◽  
Kinetic Evaluation ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Azo Initiator ◽  
Development And Validation ◽  
Kinetics Of

The oxidation of lomefloxacin (LOM) and balofloxacin (BAL) under the influence of azo initiator of radical reactions of 4,4′-azobis(4-cyanopentanoic acid) (ACVA) and H2O2 was examined. Oxidation using H2O2 was performed at room temperature while using ACVA at temperatures: 40, 50, 60 °C. Additionally, the oxidation process of BAL under the influence of KMnO4 in an acidic medium was investigated. New stability-indicating HPLC methods were developed in order to evaluate the oxidation process. Chromatographic analysis was carried out using the Kinetex 5u XB—C18 100A column, Phenomenex (Torrance, CA, USA) (250 × 4.6 mm, 5 μm particle size, core shell type). The chromatographic separation was achieved while using isocratic elution and a mobile phase with the composition of 0.05 M phosphate buffer (pH = 3.20 adjusted with o-phosphoric acid) and acetonitrile (87:13 v/v for LOM; 80:20 v/v for BAL). The column was maintained at 30 °C. The methods were validated according to the ICH guidelines, and it was found that they met the acceptance criteria. An oxidation process followed kinetics of the second order reaction. The most probable structures of LOM and BAL degradation products formed were assigned by the UHPLC/MS/MS method.

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