Degradation Kinetics Study of Alogliptin Benzoate in Alkaline Medium by Validated Stability-Indicating HPTLC Method

2016 ◽  
Vol 99 (6) ◽  
pp. 1505-1512
Author(s):  
Kunjan Bharatkumar Bodiwala ◽  
Shailesh Shah ◽  
Jeenal Thakor ◽  
Bhavin Marolia ◽  
Pintu Prajapati
Keyword(s):  
Alkaline Medium ◽  
High Performance ◽  
Degradation Kinetics ◽  
Quantitative Estimation ◽  
Solvent System ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Different Temperatures ◽  
Contour Plots ◽  
Kinetics Of

Abstract A rapid, sensitive, and stability-indicating high-performance thin-layer chromatographic method was developed and validated to study degradation kinetics of Alogliptin benzoate (ALG) in an alkaline medium. ALG was degraded under acidic, alkaline, oxidative, and thermal stress conditions. The degraded samples were chromatographed on silica gel 60F254-TLC plates, developed using a quaternary-solvent system (chloroform–methanol–ethyl acetate–triethyl amine, 9+1+1+0.5, v/v/v/v), and scanned at 278 nm. The developed method was validated per International Conference on Harmonization guidelines using validation parameters such as specificity, linearity and range, precision, accuracy, LOD, and LOQ. The linearity range for ALG was 100–500 ng/band (correlation coefficient = 0.9997) with an average recovery of 99.47%. The LOD and LOQ for ALG were 9.8 and 32.7 ng/band, respectively. The developed method was successfully applied for the quantitative estimation of ALG in its synthetic mixture with common excipients. Degradation kinetics of ALG in an alkaline medium was studied by degrading it under three different temperatures and three different concentrations of alkali. Degradation of ALG in the alkaline medium was found to follow first-order kinetics. Contour plots have been generated to predict degradation rate constant, half-life, and shelf life of ALG in various combinations of temperature and concentration of alkali using Design Expert software.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR ESTIMATION OF PITAVASTATIN CALCIUM IN BULK AND TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 47-56
Author(s):  
B. N. Suhagia ◽  
◽  
A. H. Akabari ◽  
S. A Shah ◽  
D. R Shah
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Stability Indicating ◽  
Different Temperatures ◽  
Pitavastatin Calcium ◽  
Tablet Dosage ◽  
Liquid Chromatographic

An isocratic stability-indicating reverse phase high performance liquid chromatographic diode array detection method has been developed and validated for the quantitative determination of pitavastatin calcium in the presence of its degradation products. The chromatographic separation was achieved on Phenomenex Luna C18 column (250 X 4.0 mm id, 5μm) in the isocratic mode using acetonitrilemethanol- water (35:25:40, v/v/v, pH 3 adjusted with orthophosphoric acid) as mobile phase. The drug is subjected to different accelerated stress conditions and peaks of the degradation products were well resolved from the pure drug, which indicates the specificity and stability-indicating properties of the method. The method was linear (r= 0.9998) over the concentration range of 5-30 μg/mL. The proposed method was used to investigate the degradation kinetics of PTV in acidic condition at different temperatures. Degradation of pitavastatin followed first-order kinetics, and rate constant (k), half life (t1/2), time left for 90% potency (t90) and energy of activation were calculated.

Development and Validation of Stability Indicating HPLC Method for the Determination of Impurities in the Sterile Mixture of Cefoperazone and Sulbactam

2019 ◽  
Vol 15 (7) ◽  
pp. 762-775
Author(s):  
Ramu Ivaturi ◽  
Thuttagunta Manikya Sastry ◽  
Satyaveni Sunkara
Keyword(s):  
Quantitative Estimation ◽  
Ammonium Hydroxide ◽  
Hplc Method ◽  
Forced Degradation ◽  
Buffer Solution ◽  
Solution Ph ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Abdominal Infections

Background: Cefoperazone Sulbactam injection is a cephalosporin antibiotic with a β- lactamase inhibitor used in the treatment for intra abdominal infections, Urinary track infections, surgical infections, etc. The combination is not official in any of the pharmacopeia for their content and impurities determination. Introduction: The present study involves the development of a simple, rapid, accurate, sensitive and stability indicating RP-HPLC method for the quantitative estimation of Cefoperazone Sulbactam mixture and its impurities in bulk and pharmaceutical dosage forms. Methods: 0.005 M Tetrabutyl ammonium hydroxide buffer solution pH adjusted to 6.80 and Acetonitrile combination has been used in a gradient programme with a flow rate of 1.0 ml/min. The retention time of Cefoperazone and Sulbactam were observed at around 8.5 and 19.5 minutes respectively. The UV detection was carried out at a wavelength of 230 nm. The chromatographic separation was achieved using Waters xbridge C18-150*4.6 mm, 3.5 µm HPLC column. The method has been validated according to the current International Council for Harmonization (ICH) guidelines for the method validation parameters such as Specificity, linearity, range, accuracy, precision, robustness and sensitivity. Results: The validation results indicate that the method is specific, as the known impurities and other impurities formed during the forced degradation studies were not co-eluting with the main components. Moreover, all these impurities were found to be spectrally pure, proving the stability indicating power of the method. The linearity and range of the method is in the range of 0.01-150%, highly accurate (100.2%), precise (<1%) and robust. Conclusion: The proposed method was accurate and specific for the quantitative analysis of Cefoperazone and Sulbactam and their related impurities in the sterile mixture. Hence the proposed method can be used for the quantification of impurities in routine as well as stability analysis in the development as well as quality control laboratories.

scholarly journals SIMULTANEOUS DETERMINATION OF DIPHENHYDRAMINE, EPHEDRINE, NOSCAPINE, AND GLYCEROL GLYCOLATE USING STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY: APPLICATION TO NOSCOF TABLETS

2019 ◽  
pp. 505-511
Author(s):  
PULAGURTHA BHASKARARAO ◽  
GOWRI SANKAR DANNANA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Uv Light ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters

Objective: Noscof tablet is a fixed dosage combination formulation having diphenhydramine (DH), ephedrine (ED), noscapine (NP), and glycerol glycolate (GG). A sensitive, selective, accurate, precise, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method with photodiode array detection has been developed and validated for simultaneous analysis of DH, ED, NP, and GG in bulk drug and Noscof tablets. Methods: Reversed-phase chromatographic separation and analysis of DH, ED, NP, and GG were done on an Altima C18 column with 0.01 M KH2PO4 buffer (pH 3.5) and acetonitrile (50:50%, v/v) as mobile phase at 0.8 ml/min flow rate in isocratic mode. Detection was performed at 260 nm. The method was validated in harmony with International Conference on Harmonization (ICH) guidelines. The tablet sample solution was subjected to diverse stress conditions using ICH strategy such as hydrolytic degradation (neutral - with distilled water, alkaline - with 2 N NaOH, and acidic - with 2 N HCl), oxidation (with 10% H2O2), photodegradation (exposing to UV light), and dry heat degradation (exposing to 105°C). Results: Using the above stated chromatographic conditions, sharp peaks were obtained for ED, NP, DH, and GG with retention time of 3.272 min, 4.098 min, 5.467 min, and 6.783 min, respectively. Good regression coefficient values were obtained in the range of 2–12 μg/ml for ED, 3.75–22.5 μg/ml for NP, 3.125–18.75 μg/ml for DH, and 25–150 μg/ml for GG. The quantification limits were 0.181 μg/ml, 0.187 μg/ml, 0.246 μg/ml, and 1.114 μg/ml for ED, NP, DH, and GG, respectively. The values of validation parameters are within the acceptance limits given by ICH. The ED, NP, DH, and GG showed more percent of degradation in acid condition and less percent of degradation in the neutral condition. The peaks of degradants did not interfere with the peaks of analytes. ED, NP, DH, and GG were assessed with a good percentage of the assay (near to 100%) and low percent relative standard deviation (<2%) in Noscof tablets using the proposed method. Conclusion: The stability indicating RP-HPLC method developed was suitable for quantifying ED, NP, DH, and GG simultaneously in bulk as well as in tablet formulation.

scholarly journals Degradation Kinetics of Anthocyanins in Shalgam Beverage

2019 ◽  
Vol 7 (2) ◽  
pp. 282
Author(s):  
Adnan Bozdoğan ◽  
Kurban Yaşar
Keyword(s):  
Activation Energy ◽  
Reaction Kinetics ◽  
Half Life ◽  
Degradation Kinetics ◽  
Production Method ◽  
Order Reaction ◽  
Different Temperatures ◽  
Traditional Production ◽  
Effects Of Temperature ◽  
Kinetics Of

This research was performed to elucidate the effects of temperature on the degradation kinetics of anthocyanins in shalgam beverage. Shalgam beverage was produced according to traditional production method. Then, it was kept at three different temperatures (65°C, 75°C, and 85°C) for 12 hours, and the relevant quantities of anthocyanins were determined thereafter. The research revealed that degradation of the anthocyanins was well described with a 1st-order reaction kinetics model and the R2 values varied in the range of 0.9059-0.9715. Activation energy of the reaction was determined to be 48537 Joule/mole. The half-lives of anthocyanins at 65°C and 75° C, and 85°C were found to be 138.63, 136.72, and 51.57, respectively. Compared the half-life periods at different temperatures, anthocyanins were found to be more resistant at 65°C and 75°C than at 85°C.

scholarly journals The Toxicological Testing and Thermal Decomposition of Drive and Transport Belts Made of Thermoplastic Multilayer Polymer Materials

Polymers ◽  
2020 ◽  
Vol 12 (10) ◽  
pp. 2232 ◽  
Author(s):  
Piotr Krawiec ◽  
Łukasz Warguła ◽  
Daniel Małozięć ◽  
Piotr Kaczmarzyk ◽  
Anna Dziechciarz ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Degradation Kinetics ◽  
Combustion Products ◽  
Polymer Materials ◽  
Toxic Substances ◽  
Butadiene Rubber ◽  
Different Temperatures ◽  
Increasing Temperature ◽  
In Fire ◽  
Kinetics Of

The article presents the potential impact of flat drive and transport belts on people’s safety during a fire. The analysis distinguished belts made of classically used fabric–rubber composite materials reinforced with cord and currently used multilayer polymer composites. Moreover, the products’ multilayers during the thermal decomposition and combustion can be a source of emissions for unpredictable and toxic substances with different concentrations and compositions. In the evaluation of the compared belts, a testing methodology was used to determine the toxicometric indicators (WLC50SM) on the basis of which it was possible to determine the toxicity of thermal decomposition and combustion products in agreement with the standards in force in several countries of the EU and Russia. The analysis was carried out on the basis of the registration of emissions of chemical compounds during the thermal decomposition and combustion of polymer materials at three different temperatures. Moreover, the degradation kinetics of the polymeric belts by using the thermogravimetric (TGA) technique was evaluated. Test results have shown that products of thermal decomposition resulting from the neoprene (NE22), leder leder (LL2), thermoplastic connection (TC), and extra high top cower (XH) belts can be characterized as moderately toxic or toxic. Their toxicity significantly increases with the increasing temperature of thermal decomposition or combustion, especially above 450 °C. The results showed that the belts made of several layers of polyamide can be considered the least toxic in fire conditions. The TGA results showed that NBR/PA/PA/NBR belt made with two layers of polyamide and the acrylonitrile–butadiene rubber has the highest thermal stability in comparison to other belts.

The In Vitro Degradation Kinetics of Polyurethane Prodrug Materials

2011 ◽  
Vol 399-401 ◽  
pp. 1067-1070
Author(s):  
Chun Yan Li ◽  
Cong Cong Hu ◽  
Zhi Guo Wen ◽  
Sheng Xiong Dong
Keyword(s):  
Drug Release ◽  
High Performance ◽  
Degradation Kinetics ◽  
Hplc Method ◽  
In Vitro Degradation ◽  
Erosion Mechanism ◽  
First Order ◽  
First Order Kinetics ◽  
Kinetics Of

The method of high performance liquid chromatography (HPLC) is established to determine the content of antibacterial agent — ciprofloxacin (CF) in the degradation solution of ciprofloxacin-polyurethane (CFPU) and investigate the in vitro degradation kinetics by plotting and fitting the cumulative release curves to inspect the effects of different medium and different concentrations on drug release. The results showed that the HPLC method is accurate, reliable and simple. The drug-release of CFPU was bioresponsive and could be accorded with first order kinetics. It was observed that CF was released from CFPU by a combination of diffusion and erosion mechanism, mainly in the manner of diffusion in the absence of infection while erosion mechanism in the presence of infection.

scholarly journals Stability-Indicating High-Performance Thin-Layer Chromatographic Method for Quantitative Estimation of Emtricitabine in Bulk Drug and Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Atul S. Rathore ◽  
Lohidasan Sathiyanarayanan ◽  
Kakasaheb R. Mahadik
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Bulk Drug

A simple, sensitive, precise, specific and stability indicating high-performance thin-layer chromatographic (HPTLC) method for the determination of emtricitabine both in bulk drug and pharmaceutical dosage form was developed and validated. The method employed aluminium plates precoated with silica gel G60 F254 as the stationary phase. The solvent system consisted of toluene : ethyl acetate : methanol (2 : 8 : 1, v/v/v). This solvent system was found to give compact spots for emtricitabine with value . Densitometric analysis of emtricitabine was carried out in the absorbance mode at 284 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 30–110 ng spot−1. The method was validated for precision, limit of detection (LOD), limit of quantitation (LOQ), robustness, accuracy and specificity. Emtricitabine was subjected to acid and alkali hydrolysis, oxidation, neutral hydrolysis, photodegradation and dry heat treatment. Also the degraded products peaks were well resolved from the pure drug with significantly different values. Statistical analysis proved that the method is repeatable and specific for the estimation of the said drug. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC Method

2019 ◽  
Vol 16 (1) ◽  
pp. 104-112
Author(s):  
Dharmendra Jayantibhai Prajapati ◽  
Usmangani Khalilurraheman Chhalotiya ◽  
Minesh Dahyabhai Prajapati ◽  
Jalpa Upendrabhai Patel ◽  
Jaineel Vinodrai Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Synthetic Mixture ◽  
Cancer Drug ◽  
Limit Of Quantification ◽  
Stability Indicating

Objective: An impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of Enzalutamide in bulk and synthetic mixture. Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 &amp;#177; 0. 005 and the densitometric analysis was carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture.<P&gt;

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