scholarly journals SIMULTANEOUS REVERSE-PHASE ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF GRAZOPREVIR AND ELBASVIR

2018 ◽  
Vol 11 (4) ◽  
pp. 100
Author(s):  
Madhavi S ◽  
Prameela Rani A
Keyword(s):  
Liquid Chromatography ◽  
Method Development ◽  
Degradation Products ◽  
Ultra Performance Liquid Chromatography ◽  
Main Peak ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Short Period ◽  
The Stability

 Objective: The objective of this study was to develop and validate rapid, specific, sensitive, and precise reverse-phase ultra performance liquid chromatography (RP-UPLC) method for the quantitative determination of grazoprevir and elbasvir, as there are no official monograph and no analytical method by UPLC.Methods: Chromatographic separation was achieved on a Waters Acquity UPLC HSS C18 (2.1 mm × 100 mm, 1.8 micron) column with a 45:55 (v/v) mixture of 0.1% orthophosphoric acid (pH 2.8) and acetonitrile as a mobile phase, thermostated at 30°C with a short run time of 3.0 min.Results: The retention times were 0.73 and 1.29 min for grazoprevir and elbasvir, respectively. Quantification is achieved with TUV detection at 254 nm over the concentration range of 25–150 μg/ml for grazoprevir and for elbasvir 12.5–75 μg/ml, with a correlation coefficient of 0.999 and 0.999, respectively. The developed method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity, and robustness. Forced degradation study was extended out under acidic, alkaline, oxidative, photolytic, and thermal conditions to demonstrate the stability-indicating capability of the developed UPLC method. The degradation products were well resolved from the main peak, thus proved the stability-indicating power of the method. The results of the analysis were validated statistically.Conclusion: The method is precise, accurate, linear, robust, and fast. The short retention time allows the analysis of a large number of samples in a short period of time and, therefore, should be cost-effective for routine analysis in the pharmaceutical industry.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF CABOZANTINIB IN PHARMACEUTICAL DOSAGE FORMS BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (10) ◽  
pp. 238
Author(s):  
Gorja Ashok ◽  
Sumanta Mondal
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

Objective: The proposed study aimed to develop a stability-indicating ultra-performance liquid chromatography (UPLC) method for the estimation of cabozantinib in pharmaceutical dosage form and validate the method in accordance with the International Conference on Harmonization guidelines.Methods: The optimized conditions for the developed UPLC method are Acquity UPLC Hibar C18 (100 mm × 2.1 mm, 1.7 μ) column maintained at 30°C with mobile phase consisting of 0.1% orthophosphoric acid and acetonitrile in the ratio of 55:45% v/v on isocratic mode at flow rate of 0.3 mL/ min. The sample was detected at 244 nm.Results: The retention time for cabozantinib was deemed 1.3 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 20 μg/mL and 120 μg/mL with correlation coefficient of 0.9997. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation of cabozantinib can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF APIGENIN AND LUTEOLIN FROM ACHILLEA MILLEFOLIUM LINN

2019 ◽  
pp. 169-172
Author(s):  
GOMATHY SUBRAMANIAN ◽  
S.N.MEYYANATHAN ◽  
GOWRAMMA BYRAN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Objective: A stability-indicating reverse-phase high-performance liquid chromatographic method was developed and validated for the analysis of apigenin and luteolin. The degradation behavior of apigenin and luteolin was investigated under different stress conditions as recommended by the International Conference on Harmonization (ICH). Methods: In the present study, a reversed-phase high-performance liquid chromatography method was developed and the resolution of the plant constituents was successfully achieved using Hibar Lichrospher C8 column with ultraviolet detector at a wavelength of 269 nm. The mobile phase consisted of methanol and 0.5% trifluoroacetic acid (80:20 v/v) at a flow rate of 1.0 ml/min. Both apigenin and luteolin were subjected to various stress degradation studies such as oxidation, acid and alkaline hydrolysis, and photolytic degradation. Results: The proposed method was found to be linear (1–5 μg/ml) with the linear correlation coefficient of R2=0.99. Although the degradation products of stressed conditions were not identified, the methods were able to detect the changes due to stress condition. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. Forced degradation studies on apigenin and luteolin give information about their storage and intrinsic stability conditions considering the advanced pharmaceutical aspects of formulations.

Studies on forced degradation and solid state stability of tenofovir disoproxil orotate

2021 ◽  
Vol 12 (4) ◽  
pp. 2485-2491
Author(s):  
Nageswara Rao Jakkam ◽  
Sudhakar Chintakula ◽  
Sreenivasa Rao Battula
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Regulatory System ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Drug Products ◽  
Pharmaceutical Ingredients ◽  
Ich Guidelines ◽  
Mechanism Of Degradation ◽  
The Stability

In order to develop a stability regulatory system for drug substances and degraded products, a forced degradation study is an essential part in the design of the method. As per ICH Guidelines Q1A in 1993, it was established as an essential requirement for the regulatory system to assess the stability of drugs and their degradation products under the degradation studies by force. These analytical methods are helpful in the development of stability, indicating the method by conducting the studies on forced degradation with their mechanism of degradation. Drug products by degradation and new drug substance by forced degradation conditions are more severe than a demonstration of specificity of stability indicating methods. The analytical method development is facilitated by those techniques for better understanding of (API) active pharmaceutical ingredients and (DP) drug products stability.

scholarly journals Development of a Stability Indicating Method for Simultaneous Analysis of Five Water-Soluble Vitamins by Liquid Chromatography

2018 ◽  
Vol 3 (4) ◽  
pp. 207-218 ◽  
Author(s):  
Mouloud Yessaad ◽  
Lise Bernard ◽  
Daniel Bourdeaux ◽  
Philip Chennell ◽  
Valérie Sautou
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Water Soluble ◽  
Alkaline Solutions ◽  
Array Detector ◽  
Forced Degradation ◽  
Metaphosphoric Acid ◽  
Stability Indicating ◽  
Stability Indicating Method

Abstract Background Water-soluble vitamins are often included simultaneously in pharmaceutical formulations as food complements or in parenteral nutrition mixtures. Given their sensitivity to heat, light or pH variations, it is important to study their stability using validated stability indicating methods. We thus aimed to validate a liquid chromatography (LC) stability-indicating method for the simultaneous quantification of 5 water-soluble vitamins. Methods We analyzed four water-soluble B vitamins (nicotinamide, pyridoxine, folic acid, cyanocobalamin) and ascorbic acid using a LC method with diode array detector. They were separated on a C18 stationary phase under gradient elution of solvent A [0.2 % of metaphosphoric acid in water and acetonitrile 98:2] and solvent B (100 % acetonitrile). All vitamins were subjected to forced degradation conditions and we showed that the obtained degradation products didn’t interfere with the vitamins. Results The method allows the separation of the 5 water-soluble vitamins in a 30 minute run without any interference from the breakdown products obtained with acid/alkaline solutions, hydrogen peroxide, temperature and light. It meets all the qualitative and quantitative criteria for validation with an acceptable accuracy and good linearity. Conclusions This stability-indicating method can be used for carrying out stability studies of water-soluble vitamins in pharmaceutical preparations.

scholarly journals RP-HPLC assay method development for Paracetamol and Lornoxicam in combination and characterization of oxidative degradation products of Lornoxicam

2013 ◽  
Vol 19 (4) ◽  
pp. 471-484
Author(s):  
Pritam Jain ◽  
Miketa Patel ◽  
Amar Chaudhari ◽  
Sanjay Surana
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Oxidative Degradation ◽  
Assay Method ◽  
Forced Degradation ◽  
Control Analysis ◽  
Reverse Phase ◽  
Solution Form ◽  
Forced Degradation Studies ◽  
Degradation Studies

A simple, specific, accurate and precise reverse phase high pressure liquid chromatographic method has been developed for the simultaneous determination of Paracetamol and Lornoxicam from tablets and to characterize degradation products of Lornoxicam by reverse phase C18 column (Inertsil ODS 3V C-18, 250 x 4.6 mm, 5 ?). The sample was analyzed using Buffer (0.02504 Molar): Methanol in the ratio of 45:55, as a mobile phase at a flow rate of 1.5 mL/min and detection at 290 nm. The retention time for Paracetamol and Lornoxicam was found to be 2.45 and 9.40 min respectively. The method can be used for estimation of combination of these drugs in tablets. The method was validated as per ICH guidelines. The linearity of developed method was achieved in the range of 249.09 - 747.29 ?g/mL (r2=0.9999) for Paracetamol and 4.0125 - 12.0375 ?g/mL (r2=0.9999) for Lornoxicam. Recoveries from tablets were between 98 and 102%. The method was validated with respect to linearity, accuracy, precision, robustness and forced degradation studies which further proved the stability-indicating power. During the forced degradation studies lornoxicam was observed to be labile to alkaline hydrolytic stress and oxidative stress (in the solution form). However, it was stable to the acid hydrolytic, photolytic and thermal stress (in both solid and solution form). The degraded products formed were investigated by electrospray ionization (ESI) time-of-flight mass spectrometry, NMR and IR spectroscopy. A possible degradation pathway was outlined based on the results. The method was found to be sensitive with a detection limit of 0.193 ?g/ml, 2.768 ?g/ml and a quantitation limit of 0.638 ?g/ml, 9.137 ?g/ml for lornoxicam and paracetamol, respectively. Due to these attributes, the proposed method could be used for routine quality control analysis of these drugs in combined dosage forms.

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.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING REVERSE-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF POTENTIAL DEGRADATION PRODUCTS OF REGADENOSON FROM ITS PARENTERAL DOSAGE FORM

2018 ◽  
Vol 11 (8) ◽  
pp. 277
Author(s):  
Murlidhar V Zope ◽  
Rahul M Patel ◽  
Ashwinikumari Patel ◽  
Samir G Patel
Keyword(s):  
Liquid Chromatography ◽  
Degradation Product ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method ◽  
Injectable Dosage

Objective: The objective was to develop and validate the stability indicating reverse-phase high-performance liquid chromatography method for the quantification of potential degradation products of regadenoson (REGA) from its injectable dosage form.Methods: YMC-PAK ODS AQ, 150 mm × 4.6 mm, 3 μm composed with hydrophobic high carbon loading and a relatively hydrophilic surface chemically bonded to porous silica particles column was used with the temperature maintained at 40°C. Mobile phase A composed of 0.1% triethylamine buffer having pH 4.5 while mobile phase B is 100 % acetonitrile was used for gradient elution with 1.5 ml/min as a flow rate. The wavelength used for quantification was 245 nm and 20 μl as an injection volume. The suitability of the method has been checked and validated according to the International Council for Harmonization (ICH) guidelines for different parameters, namely, specificity, linearity, accuracy, precision, limit of quantification (LOQ), Limit of detection (LOQ), and robustness studies.Results: The resolution between REGA and its two-degradation product is >8.0 for all pairs of components. The high correlation coefficient (r2>0.990) values are for drug and all potential degradation products from LOQ to 150% of specification limits for impurities calculated based on the maximum daily dose of REGA. LOQ for the drug as well as each degradation product is <0.02% w/w. The % relative standard deviation (RSD) for precision and intermediate precision is in the range of 0.17–0.89, and % RSD for precision at LOQ is 0.86–2.35. The % RSD for robustness study is maximum 2.59.Conclusion: The developed method can quantify the specified and unknown degradation products from 0.1% in the injectable dosage form which indicates that method is sensitive. Method fulfills the ICH criteria for its different validation parameters and demonstrates that the developed analytical method is highly specific, precise, and robust and would have a great value when applied in quality control and stability studies for REGA injection.

Stability-indicating LC method for the determination of cephalothin in lyophilized powder for injection

2014 ◽  
Vol 6 (12) ◽  
pp. 4437-4445 ◽  
Author(s):  
Karen de Souza Rugani ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Antimicrobial Compound ◽  
Reversed Phase Liquid Chromatography ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Phase Liquid

A stability-indicating gradient reversed phase liquid chromatography (RP-LC) method has been developed for the quantitative determination of cephalothin (CET), an antimicrobial compound, in the presence of its impurities and degradation products generated from forced degradation studies.

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