scholarly journals Development and Validation of Stability Indicating RP-HPLC Assay Method for Mefenamic Acid

2019 ◽  
Vol 31 (3) ◽  
pp. 656-660
Author(s):  
Adison Fernandes ◽  
P.N. Sanjay Pai
Keyword(s):  
Thermal Stress ◽  
Mefenamic Acid ◽  
Degradation Products ◽  
Research Work ◽  
Stress Conditions ◽  
Assay Method ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Photodiode Array Detector ◽  
The Stability

The present research work was carried out to evaluate the stability behaviour of mefenamic acid under ICH Q1A (R2) recommended stress conditions. The drug was subjected to hydrolytic, oxidative, photolytic and thermal stress conditions. The drug was found susceptible to degradation under oxidative stress condition but was stable under hydrolytic, photolytic and thermal stress conditions. A total two degradation products were formed, which were separated using HPLC. The chromatographic separation was carried out on Sunfire ODS C-18 (250 × 4.6 mm, 5 μm) column. Optimum resolution was obtained using ammonium dihydrogen phosphate buffer (10 mM, pH 4) and acetonitrile programmed in isocratic elution mode in the ratio of 45:55 v/v at 225 nm using photodiode array detector at a flow rate of 1 mL/min. The designed method was validated as per ICH Q2 (R1) guidelines. The response of drug was linear in the concentration range of 10-100 μg/mL (R2 = 0.9998). The method was found specific, precise and accurate. The mean accuracy was found to be 100.46 %. The developed method was successfully applied for the analysis of marketed formulation.

scholarly journals Stability-Indicating RP-HPLC Method for Assay of Silver Lactate

2011 ◽  
Vol 8 (2) ◽  
pp. 483-490
Author(s):  
V. Srinivasan ◽  
H. Sivaramakrishnan ◽  
B. Karthikeyan
Keyword(s):  
Thermal Stress ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Stress Conditions ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

A simple, economic and time-efficient stability-indicating, reverse-phase high-performance liquid chromatographic (RP-HPLC) method has been developed for analysis of silver lactate in the presence of degradation products generated by decomposition. When silver lactate was subjected to acid hydrolysis, base hydrolysis, oxidative, photolytic, humidity and thermal stress, degradation was observed during base hydrolysis, oxidation, humidity and thermal stress. The drug was found to be stable to other stress conditions. Successful chromatographic condition of the drug from the degradation products formed under stress conditions was achieved on a phenomenex Gemini column with potassium dihydrogen phosphate buffer, pH adjusted to 2.2 with orthophosphoric acid, as mobile phase. The method was validated for linearity, precision, specificity and robustness and can be used for quality-control during manufacture and assessment of the stability of samples of silver lactate. To the best of our knowledge, a validated stability-indicating LC assay method for silver lactate based on lactic acid is reported for the first time.

scholarly journals Characterization and toxicity evaluation of degradation products of febantel

2020 ◽  
Vol 6 (1) ◽  
Author(s):  
Anand A. Mahajan ◽  
Amey M. Marathe ◽  
Suvarna S. Jarande ◽  
Raghuvir Pissurlenkar ◽  
Vandana T. Gawande
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Gradient Elution ◽  
Stress Conditions ◽  
Array Detector ◽  
Forced Degradation ◽  
Photodiode Array Detector ◽  
Positive Mode ◽  
In Silico Toxicity ◽  
The Stability

Abstract Background The aim of the present work was to determine potential toxicity of degradation products of febantel generated under different stress conditions mentioned in guideline Q1A (R2) laid down by International Council for Harmonization (ICH). The stability behavior of febantel was studied by subjecting it to hydrolytic, oxidative, photolytic and thermal forced degradation conditions. Results Five degradation products (DPs) were observed which were resolved using high-performance liquid chromatography (HPLC) and characterized by LC-MS/MS using positive mode of electrospray ionization. The chromatographic separation was carried out on Hypersil® BDS C18 (150 × 4.6 mm, 5 μm) column. Optimum resolution was obtained using ammonium formate buffer (10 mM, pH 3.5) and acetonitrile programmed in gradient elution mode at 281.0 nm using photodiode array detector. Conclusion The drug was found susceptible to degradation under all the stress conditions except thermal and oxidative stress. Five major unknown degradation products DP–I, DP–II, DP–III, DP–IV, and DP–V generated under photolytic, alkali, and acidic stress condition were identified and characterized by LC-MS/MS. The drug and identified degradation products were screened for prediction of in-silico toxicity using software viz. Swiss ADME, OSIRIS Property Explorer and Pro Tox II which indicated overall no toxicological concerns. Graphical abstract

Stability Indicating RP-UPLC Photo-Diode Array based Method for Determination of Edoxaban Tosylate

2020 ◽  
Vol 5 (3) ◽  
pp. 273-276
Author(s):  
D.M. Patel ◽  
B. Rana ◽  
S. Maru ◽  
A.J. Vyas ◽  
A.B. Patel ◽  
...  
Keyword(s):  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Ultra Performance Liquid Chromatography ◽  
Reversed Phase ◽  
Assay Method ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Stress Studies

The objective of the current study was to develop a specific, precise, accurate and robust gradient stability indicating reversed-phase ultra performance liquid chromatography (RP-UPLC-PDA) assay method and validated for determination of edoxaban tosylate in API. Gradient separation was achieved on an acquity UPLC BEH C18 column (50 mm, 2.1 mm and 1.7 μm) column using mobile phase of acetoitrile:20 mM potassium dihydrogen phosphate, pH 3.0 ± 0.05 adjust with OPA at flow rate of 0.6 mL/min, the injection volume was 1 μL and the detection was carried out of 289 nm by using photodiode array detector. The drug was subjected to oxidation, hydrolysis, photolysis, and heat to apply stress condition. The method was linear in the drug concentration range of 100-300 μg/mL with correlation coefficient of 0.999. Degradation products produced as a result of stress studies did not interfere with detection of edoxaban tosylate and the assay, thus developed stability indicating method can be used for routine analysis in pharmaceutical industry.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

A New, Rapid and Simple RP-HPLC Method for Stability Quantification of a Protease Inhibitor in Tablets

2021 ◽  
Author(s):  
Rochele Cassanta Rossi ◽  
Josué Guilherme Lisbôa Moura ◽  
Vanessa Mossmann ◽  
Patrícia Weimer ◽  
Pedro Eduardo Fröehlich
Keyword(s):  
Quality Control ◽  
Protease Inhibitor ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Control Analysis ◽  
Quality Control Laboratory ◽  
The Stability

Abstract Fosamprenavir calcium is a protease inhibitor widely used in the treatment and prevention of human immunodeficiency virus and acquired immunodeficiency syndrome. This protease inhibitor serves as a prodrug of amprenavir, offering better oral bioavailability. Although this drug was approved by the FDA in 2003, there are few methods established for quantifying the stability for quality control analysis of fosamprenavir-coated tablets. The purpose of the study was to develop and validate a method for determining the stability of fosamprenavir-coated tablets (Telzir®) that may be applied by any quality control laboratory. Chromatographic separation was performed using a Vertical RP-18 column programmed to run a gradient elution with sodium acetate buffer and acetonitrile. Flow rate was 1.2 mL min−1 for a total run time of 15 min. Ultraviolet detection was set at 264 nm and the use of a photodiode array detector in scan mode allowed selectivity confirmation by peak purity evaluation. The analyte peak was found to be adequately separated from degradation products generated during forced degradation studies. Thus, the proposed method was found to accurately indicate stability and was sufficient for routine quantitative analysis of fosamprenavir in coated tablets without interference from major degradation products and excipients.

Novel Determination of Anti-Hypertensive Combination; Benidipine Hydrochloride and Nebivolol Hydrochloride by High Performance Chromatographic Method

2021 ◽  
pp. 5433-5438
Author(s):  
V.L.N. Balaji Gupta Tiruveedhi ◽  
Venkateswara Rao Battula ◽  
Kishore Babu Bonige ◽  
Tejeswarudu B.
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Research Work ◽  
Hplc Method ◽  
Assay Method ◽  
Injection Quantity ◽  
Relative Standard ◽  
Nebivolol Hydrochloride ◽  
Concentration Series

This research work was designed to establish and validate a novel stability indicating RP-HPLC method for the combined determination of Benidipine hydrochloride (BHE) and Nebivolol hydrochloride (NHE) in bulk and tablets, dependent on ICH guidelines.The assay method to analyse BHE and NHE was optimized with isocratic elution using acetonitrile: 0.1M acetate buffer (45:55, pH 5.1), Lichrospher ODS RP-18 column and flow pace of 1 ml/min. Total time for single run was 14 min. The injection quantity was 20μl, and was detected at 249nm. The method was verified on a concentration series of 1.25-10μg/ml (NHE) and 1.0-10μg/ml (BHE) for precision, accuracy and linearity. The LOD values were 0.059µg/ml and 0.028µg/ml for NHE and BHE, respectively. The LOQ values were 0.196µg/ml for NHE and 0.094µg/ml for BHE. The recovery percentages were 98.60-100.11% (BHE) and 98.94-101.50% (NHE) with relative standard deviation 0.250-0.694% (BHE) and 0.183-0.400% (NHE). The method was also observed to be efficient, and was sufficiently specific to measure BHE and NHE in the presence of stress-produced degradation products.

scholarly journals Validation of developed method by RP-HPLC for estimation of Prasugrelin human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 13 (1) ◽  
pp. 65-75
Author(s):  
Kumar S. Ashutosh ◽  
Debnath Manidipa ◽  
Rao J.V.L.N. Seshagiri ◽  
Sankar D. Gowri
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
The Stability

This paper is concern with a reverse phase high performance liquid chromatography (RP-HPLC) bio-analytical method development and validation for Prasugrel in human plasma using photo diode array detector (PDA detector). The HPLC separation was carried out in an isocratic mode on an X-Terra C18 column (4.6 x 150 mm; 5 μm) with a mobile phase consisting of potassium dihydrogen phosphate [pH 3.0] and acetonitrile in the ratio of 30:70 v/v at a flow rate of 1.0 mL/min. The run time was maintained for 5 mins and the detection was monitored at 210 nm. The percentage recovery was found 99.61-100.06 in human plasma. This reveals that the method is quite accurate. The linearity was found 15-40 μg/mL in human plasma. The inter-day and intra-day precision in plasma was found within the limits. The lower limit of quantification (LLOQ) obtained by the proposed method was 0.05 μg/mL. The percentage relative standard deviation (%RSD) obtained for the drug spiked in plasma for stability studies were less than 2 %.Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 65-75

STABILITY INDICATING ASSAY METHOD OF SIROLIMUS USING HPLC AND SEPARATION OF ACID DEGRADANT BY HPTLC

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (04) ◽  
pp. 48-55
Author(s):  
S. Jadhav ◽  
◽  
P. Pisal ◽  
M. Mahajan
Keyword(s):  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Oxidation Stress ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
The Given ◽  
Stressed Sample

A stability indicating RP-HPLC method has been developed and subsequently validated for Sirolimus. The proposed RP-HPLC method utilizes Phenomenex, C18, 3 μm, 4 mm x 150 mm column, mobile phase consisting of acetonitrile and water (65:35 V/V) and UV detection at 277 nm using a photodiode array detector in the stressed sample chromatograms. Crushed sirolimus tablets were exposed to thermal, photolytic, aqueous and oxidation stress conditions and stressed samples were analysed by the proposed method. Peak homogeneity data of the drug peaks were obtained using photodiode array detector. The stressed sample chromatograms demonstrated the specificity of the method for their estimation in presence of degradants. 99.66% degradation was observed in acid degradation study. on the other hand, no degradation was observed in aqueous condition. The given method was linear over a range of 0.1566 mg/mL to 0.4699 mg/mL. The mean recovery was found to be 99.23%. Acid degradant was separated by HPTLC and spectroscopic analysis was performed for the same.

scholarly journals Isolation and Structural Characterization of Degradation Products of Aceclofenac by HPLC, HRMS and 2D NMR

2019 ◽  
Vol 31 (4) ◽  
pp. 851-854
Author(s):  
Santhosh Guduru ◽  
V.V.S.R.N. Anji Karun Mutha ◽  
B. Vijayabhaskar ◽  
Muralidharan Kaliyaperumal ◽  
Raghu Babu Korupolu ◽  
...  
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Acid Stress ◽  
2D Nmr ◽  
Stress Conditions ◽  
Preparative Hplc ◽  
Mass Spectral ◽  
2D Nmr Spectra ◽  
The Stability

The stability of aceclofenac under stress conditions was assessed to identify the degradation products. So, it was subjected to stress conditions like acid, base and oxidation, according to ICH guideline Q1A (R2). One degradation product formed when the drug was subjected to acid stress. Three degradation products were formed during the basic stress condition. The drug substance was found to be stable to oxidative stress. The degradants formed during the stress were separated on a C-18 column using gradient preparative HPLC elution. The only product (DP-2) formed during the acid stress and this one is same as of one of the three degradation products (DP-1, DP-2, DP-3) were formed during base stress. 1D and 2D NMR spectra and mass spectral analysis supported the proposed structures for the products. The products DP-2 and DP-3 have been reported earlier but this is the first report of product DP-1 as a degradation product of aceclofenac.

scholarly journals Development and Validation of a Novel Stability-Indicating Reversed-Phase Ion-Pair Chromatographic Method for the Quantitation of Impurities in Marbofloxacin Tablets

2018 ◽  
Vol 101 (4) ◽  
pp. 1021-1029
Author(s):  
Priyanka Maheshwari ◽  
Neelima Shukla ◽  
Manish Kumar Dare
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Ion Pair ◽  
Stress Conditions ◽  
Main Peak ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
The Stability

Abstract A stability-indicating isocratic reversed-phase ion-pair chromatographic method was designed for the separation of impurities in the presence of degradation products. Marbofloxacin tablets and a placebo were exposed to the stress conditions of oxidative, acid, base, humidity, thermal, and photolytic degradation. Significant and moderate degradation was observed in acidic and oxidative stress conditions, respectively. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating analytical method. The method was developed by using an XTerra RP18 3.5 μm (150 × 4.6 mm) column, with the mobile phase containing a mixture of buffer (pH 2.5)–methanol–glacial acetic acid (77 + 23 + 0.5, v/v). The flow rate of the mobile phase was 1.2 mL/min, with a column oven temperature of 40°C and a detection wavelength of 315 nm. The proposed method met Veterinary International Conference on Harmonization requirements and was successfully used for impurity quantitation in marbofloxacin tablets.

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