scholarly journals A Validated Stability-Indicating Liquid Chromatographic Method for the Determination of Lorcaserin and Related Impurities in DRUG Substance Supported by Quality by Design

2020 ◽  
Vol 58 (7) ◽  
pp. 661-671
Author(s):  
Dattatraya V Wani ◽  
Santosh N Mokale
Keyword(s):  
Quality By Design ◽  
Stress Condition ◽  
Ammonia Solution ◽  
Solution Ph ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Impurities ◽  
Stability Indicating Method ◽  
Liquid Chromatographic

Abstract Lorcaserin (LOR) is selective and potent antiobesity drug that targets the activation of the serotonin 5HT2C receptor. Here a novel, specific, sensitive stability indicating method was developed and validated for the quantitative determination of LOR and its process-related impurities using quality by design principles. By applying experimental design, the authors examine the multifactorial effect of parameters on the critical resolution pair and generated design space representing the robust design. LOR was subjected to stress condition and found stable at all condition, only found significant degradation at oxidative stress condition. The chromatographic separation of degradation product and its process-related impurities were achieved on a Phenomenox Luna phenyl-hexyl column (150 × 4.6 mm × 5 μm), with mobile phase consisting of 10 mM ammonium formate containing 0.1% ammonia solution; pH adjusted to 2.8 with trifluoroacetic acid as solvent A and methanol/acetonitrile (5/95) as solvent B delivered with gradient program at a flow rate of 1.0 mL/min, column temperature was maintained at 25°C and analytes were monitored at 220 nm. The injection volume was 5 μL. The developed RP-LC method was validated and found linear, accurate, specific, selective, precise and robust. The structure of impurities was confirmed by direct mass analysis.

Analytical Quality by Design Approach for a Stability-Indicating Method to Determine Apixaban and Its Related Impurities

2019 ◽  
Vol 83 (1) ◽  
pp. 65-75 ◽  
Author(s):  
Jéssica B. Ellwanger ◽  
Nathalie Ribeiro Wingert ◽  
Nadia Maria Volpato ◽  
Cássia Virginia Garcia ◽  
Elfrides E. S. Schapoval ◽  
...  
Keyword(s):  
Quality By Design ◽  
Design Approach ◽  
Analytical Quality ◽  
Stability Indicating ◽  
Related Impurities ◽  
Stability Indicating Method ◽  
Quality By Design Approach

scholarly journals Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Fahimeh Sadeghi ◽  
Latifeh Navidpour ◽  
Sima Bayat ◽  
Minoo Afshar
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Ph ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r2=0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations.

scholarly journals Development and validation of stability indicating method for determination of sodium citrate in pediatric cough syrup

2020 ◽  
Vol 8 (2) ◽  
pp. 213-223
Author(s):  
Abdrhman Mahmoud Gamil ◽  
Mohamed Awad al-lkareem Hamad
Keyword(s):  
Sodium Citrate ◽  
Degradation Products ◽  
Base Hydrolysis ◽  
Column Temperature ◽  
Stability Indicating ◽  
Spectrophotometric Methods ◽  
End Point ◽  
Regulatory Affairs ◽  
Stability Indicating Method

Sodium Citrate is widely used in analytical and food processes. It is used in various medical applications as anticoagulant in blood transfusion process and bladder washout. It is used in cough preparation as mucolytic. There are many methods for determination of Sodium Citrate in different preparations. Some of which use spectrophotometric methods, others used HPLC methods. The USP method uses titration and determining the end point potentionometrically. Many arguments take place between the Drug Regulatory Affairs and manufacturers regarding the appearance of the colour at the end point. The objective of this study is to develop and validate a simple, easy and precise HPLC stability indicating method for routine work and to be submitted to the Drug Regulatory Affairs. Chromatographic system with detector PDA at 210nm is utilized, Reprosil-XR C18, 250 mm×4 mm, 5 µm column is used. Column temperature 300C and flow rate of 1 ml/min. A clear peak of acceptable purity at 3.38 min retention time appears. The method is subjected to thermal stress, acid and base hydrolysis at extreme pH and forced oxidation. The result is that there is no interference of degradation products with the substance peak. The method is then subjected to validation study according to the ICH guidelines. The method comply the specificity, precision, linearity, accuracy and robustness acceptable criteria. Thus, the method satisfies the stability indicating method and validation requirements that it can be submitted to the Drug Regulatory Affairs and used in QC routine activities and stability studies.

Stability indicating assay method for determination of Febuxostat by RP-HPLC

2021 ◽  
Vol 01 ◽  
Author(s):  
Ramanlal N. Kachave ◽  
Pragati B. Mandlik ◽  
Akshay G. Mundhe
Keyword(s):  
Limit Of Detection ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Limit Of Quantitation

Objective: A simple, rapid, precise and accurate RP-HPLC stability indicating method was developed and validated for estimation of Febuxostat in bulk drug and marketed tablet formulation. Methods: The chromatographic separation was achieved on Agilent C18 (250 x 4.6mm, 5 µm) using solvent 15 mM ammonium acetate buffer (pH 4.8) and acetonitrile (30:70 v/v) as a mobile phase at flow rate of 1 mL/min and at ambient column temperature analysis were carried out at detection wavelength 315nm. Result: The method was validated for linearity, precision, accuracy, specificity, LOD and LOQ, and robustness. The linearity was studied in the concentration range of 5-25 µg/mL and correlation coefficient was found to be 0.999. The limit of detection and limit of quantitation were found to be 0.37 µg/mL and 1.13 µg/mL. Febuxostat was subjected to stress condition of degradation including acidic, alkaline, oxidation, photolytic and thermal degradation. Febuxostat is more sensitive toward acidic condition than oxidation and less sensitive towards alkaline, thermal and photolytic degradation. Conclusion: The method is simple, reliable, sensitive and precise which could separate the drug and their degraded product formed under various stress conditions, thus it can be employed as stability indicating method for the determination of FBX in bulk and pharmaceutical dosage form.

scholarly journals STABILITY INDICATING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS DETERMINATION OF PHENYLEPHRINE HYDROCHLORIDE, CHLORPHENIRAMINE MALEATE, PARACETAMOL, GUAIPHENESIN AND BROMHEXINE HYDROCHLORIDE IN BULK AND PHARMACEUTICAL FORMULATION

2019 ◽  
pp. 284-292
Author(s):  
PRASANTHI CHENGALVA ◽  
MADHAVI KUCHANA
Keyword(s):  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Acid Base ◽  
Chlorpheniramine Maleate ◽  
Column Temperature ◽  
Phenylephrine Hydrochloride ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Liquid Chromatographic

Objective: The objective of the present study is to develop simple, rapid, sensitive, accurate and economic stability-indicating ultra-performance liquid chromatographic (UPLC) method for the simultaneous quantification of phenylephrine hydrochloride, chlorpheniramine maleate, paracetamol, guaiphenesin and bromhexine hydrochloride in bulk and tablet dosage form. Methods: The separation of drugs in the chromatographic column was accomplished on Hibar C18 (100 mm x 2.1 mm, 1.6 µm) column at a detection wavelength of 220 nm. The mobile phase was a combination of sodium phosphate monobasic monohydrate buffer (pH was adjusted to 3.5 with orthophosphoric acid) and acetonitrile in the ratio of 70:30 % v/v which was pumped at a flow rate of 0.3 ml/min. The column temperature was maintained at 30 °C and the injection volume was 0.3 µl. Forced degradation studies of drugs were carried out using acid, base, peroxide, light and heat. Results: All the five drugs have been eluted within 3 min. The retention times were found to be 0.834 min, 1.199 min, 1.600 min, 1.979 min and 2.525 min for phenylephrine, chlorpheniramine maleate, paracetamol, guaiphenesin and bromhexine respectively. The correlation coefficient (r2) was found to be 0.999 for all the drugs. The recovery levels were found to be in the range of 99.17 % to 100.69 %. RSD values of drugs were found to be below 2 %. The results of limit of detection and quantitation specified the sensitivity of the developed method. Significant degradation of drugs as a result of stress studies was found in acid, base and peroxide, but they were slightly degraded in photolytic and thermal conditions. The method has effectively resolved the degraded products. All the validation parameters were found to be within the limits according to International Conference on Harmonization (ICH) guidelines. Conclusion: A simple and rapid UPLC method was established for the determination of five drugs. Hence, the proposed method can be employed for the quality control of specified drugs in bulk and pharmaceutical formulation even in the presence of degradation products.

scholarly journals Liquid Chromatographic Determination of Pyrantel Tartrate in Medicated Formulations

2003 ◽  
Vol 86 (5) ◽  
pp. 882-887
Author(s):  
Joyce A Konrardy ◽  
Mary A Burner ◽  
Tommy W Garner ◽  
Mark A Litchman ◽  
Gregory K Webster
Keyword(s):  
Chromatographic Determination ◽  
Official Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Liquid Chromatographic Determination ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Aoac Official Method ◽  
Pyrantel Tartrate

Abstract The validation of a novel liquid chromatographic (LC) method for the determination of pyrantel tartrate in feed is presented. The method provides a significant improvement over the efficiency and precision of AOAC Official Method 978.30. The method was shown to be accurate, precise, linear, and robust for medicated articles. Unlike the official method, the LC method was shown to be a superior stability-indicating method. After the method was validated by using laboratory blends, the effectiveness of the method was demonstrated with marketed product as well.

scholarly journals Stability Indicating Method for Simultaneous RP HPLC Determination of Camylofin Dihydrochloride and Nimesulide in Pharmaceutical Preparations

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Rajeev Kumar R. Singh ◽  
Manapragada V. Rathnam ◽  
Sangeeta J. Singh ◽  
Raju V. K. Vegesna
Keyword(s):  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Control Analysis ◽  
Solution Stability ◽  
Buffer Solution ◽  
Solution Ph ◽  
Column Temperature ◽  
Stability Indicating

A simple, fast, and precise reversed phase high-performance liquid chromatographic method has been developed for the simultaneous determination of camylofin dihydrochloride and nimesulide using caffeine as an internal standard. The stability indicating capability of the method was proved by subjecting the drugs to stress conditions as per ICH-recommended test conditions. Separation was achieved using Varian Chromspher 5 C18 column (250 mm × 4.6 mm, 5 μm) as stationary phase with a mobile phase comprising of buffer solution pH 5.0 : methanol (600 : 400, v/v) at a flow rate of 1.0 mL min−1, column temperature of 30∘C and UV detection at 220 nm. The retention time of caffeine, camylofin dihydrochloride, and nimesulide was about 5.0 min, 6.1 min, and 12.7 min, respectively. The proposed method was validated for linearity, accuracy, precision, sensitivity, robustness and solution stability. Linearity, accuracy, and precision were found to be acceptable over the ranges of 250–750 μg mL−1 for Nimesulide and 125–375 μg mL−1 for camylofin dihydrochloride. The test solution was found to be stable for 72 h. It can be conveniently adopted for routine quality control analysis.

Sign in / Sign up

Export Citation Format

Share Document