HPLC and HPLC/MS/MS Studies on Stress, Accelerated and Intermediate Degradation Tests of Antivirally Active Tricyclic Analog of Acyclovir

2015 ◽  
Vol 98 (5) ◽  
pp. 1240-1247 ◽  
Author(s):  
Monika A Lesniewska ◽  
Paweł Dereziński ◽  
Agnieszka Klupczyńska ◽  
Zenon J Kokot ◽  
Tomasz Ostrowski ◽  
...  
Keyword(s):  
Solid Phase ◽  
Degradation Products ◽  
Strong Acid ◽  
Good Clinical Practice ◽  
Degradation Behavior ◽  
Acid Base ◽  
Dry Heat ◽  
Rp Hplc ◽  
Tricyclic Analog ◽  
The Stability

Abstract The degradation behavior of a tricyclic analog of acyclovir [6-(4-MeOPh)-TACV] was determined in accordance with International Conference on Harmonization guidelines for good clinical practice under different stress conditions (neutral hydrolysis, strong acid/base degradation, oxidative decomposition, photodegradation, and thermal degradation). Accelerated [40 ± 2°C/75% ± 5% relative humidity (RH)] and intermediate (30 ± 2°C/65% ± 5% RH) stability tests were also performed. For observation of the degradation of the tested compound the RP-HPLC was used, whereas for the analysis of its degradation products HPLC/MS/MS was used. Degradation of the tested substance allowed its classification as unstable in neutral environment, acidic/alkaline medium, and in the presence of oxidizing agent. The tested compound was also light sensitive and was classified as photolabile both in solution and in the solid phase. However, the observed photodegradation in the solid phase was at a much lower level than in the case of photodegradation in solution. The study showed that both air temperature and RH had no significant effect on the stability of the tested substance during storage for 1 month at 100°C (dry heat) as well as during accelerated and intermediate tests. Based on the HPLC/MS/MS analysis, it can be concluded that acyclovir was formed as a degradation product of 6-(4-MeOPh)-TACV.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for Determination of Atomoxetine Hydrochloride in Tablets

2010 ◽  
Vol 93 (4) ◽  
pp. 1207-1214 ◽  
Author(s):  
Sejal K Patel ◽  
Natvarlal J Patel
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Acid Base ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Wet Heat

Abstract This paper describes the development of a stability-indicating RP-HPLC method for the determination of atomoxetine hydrochloride (ATX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of acid, base, oxidation, wet heat, dry heat, and photodegradation. In stability tests, the drug was susceptible to acid, base, oxidation, and dry and wet heat degradation. It was found to be stable under the photolytic conditions tested. The drug was successfully separated from the degradation products formed under stress conditions on a Phenomenex C18 column (250 4.6 mm id, 5 m particle size) by using acetonitrilemethanol0.032 M ammonium acetate (55 + 05 + 40, v/v/v) as the mobile phase at 1.0 mL/min and 40C. Photodiode array detection at 275 nm was used for quantitation after RP-HPLC over the concentration range of 0.55 g/mL with a mean recovery of 100.8 0.4 for ATX. Statistical analysis demonstrated that the method is repeatable, specific, and accurate for the estimation of ATX. Because the method effectively separates the drug from its degradation products, it can be used as a stability-indicating method.

scholarly journals Fasten, simple, and specific stability of the avant-garde RP-HPLC method for estimation and validation of nystatin in pharmaceutical formulations

2019 ◽  
Vol 10 (4) ◽  
pp. 3717-3727
Author(s):  
Dawood CH. Al-Bahadily ◽  
Rasool Chaloob ◽  
Kulood H. Oudah ◽  
H. N. K. AL-Salman ◽  
Falah Hassan Shari ◽  
...  
Keyword(s):  
Flow Rate ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Avant Garde ◽  
Rp Hplc ◽  
Specificity And Sensitivity ◽  
Stress Degradation ◽  
The Stability

In this study, a simple and reliable stability-indicating RP-HPLC method was developed and validated for the analysis of Nystatin in the pharmaceuticals. The chromatographic separation was performed in the isocratic mode on an Ion Pac column; Arcus EP‑C18; 5μm, 4.6×250 mm, 30 °C) using a mobile phase consisting of ammonium acetate 0.05 M buffer/ Methanol mixture (30:70) and a flow-rate of 1.0 mL/min with UV detection at 305 nm. The flow rate was set at 1.0 mL/min. The HPLC analysis method was validated in terms of linearity, precision, accuracy, specificity, and sensitivity, according to International Conference on Harmonization (ICH) guidelines. The results indicated that the retention time was 8 min, and no interferences were observed from the formulation excipients and stress degradation products.  The specificity, linearity, precision, accuracy, LOD, and LOQ of the method were validated. The method was linear over the range of 5–500 μg/mL with an acceptable correlation coefficient (R2 = 0.9996). The method’s limit of detection (LOD) and quantification (LOQ) were 0.01 and 0.025 μg/mL, respectively. The results indicate that this validated method can be used as an alternative method for the assay of nystatin. This validated HPLC method could be used for routine analysis, quality control, and the stability of analysis of Nystatin formulations.

scholarly journals Degradation study of stevioside using RP-HPLC and ESI-MS/MS

2018 ◽  
Vol 14 (1-2) ◽  
pp. 138-141 ◽  
Author(s):  
Yohanes Martono ◽  
Abdul Rohman ◽  
Sudibyo Martono ◽  
Sugeng Riyanto
Keyword(s):  
Degradation Products ◽  
Stress Factors ◽  
Base Hydrolysis ◽  
Esi Ms ◽  
Rp Hplc ◽  
Base Solution ◽  
Acid And Base ◽  
Dry Heating ◽  
H2o2 Oxidation ◽  
The Stability

Stevioside is very potential to be an antidiabetic pro-drug. In processing, the active ingredient may be degraded. This research conducted a study of the degradation of stevioside on several stress factors such as acid and base hydrolysis; exposure to UV rays, thermal heating and oxidation using RP-HPLC. The degradation products were identified using ESI-MS/MS. Hydrolysis of acid-base solution and exposure to UV254 nm rays caused the breakdown of glycoside bonds in the analyte. Stevioside was unstable in dry heating at 105oC for 48 hours due to degradation of 91%. Stevioside was oxidized under H2O2 oxidation for 48 hours. Based on the ESI-MS/MS analysis, the identified stevioside degradation products were [M-H] ̶ with m/z = 803 as stevioside; [M-H] ̶ with the value of m/z = 641 as steviolbioside; [M-H] ̶ with m/z = 479 as steviolmonoside; [M-H] ̶ with m/z = 317 as steviol. Termination of glucose was characterized by fragmentation [M-162] ̶.Our study provides a basic view on the stability and degradation characteristics of stevioside, and demonstrates the formation of degradation products.

scholarly journals Stability-Indicating RP-HPLC Method Development and Validation for Duloxetine Hydrochloride in Tablets

2010 ◽  
Vol 93 (1) ◽  
pp. 123-132 ◽  
Author(s):  
Sejal K Patel ◽  
Natavarlal J Patel ◽  
Arun M Prajapati ◽  
Dipti B Patel ◽  
Satish A Patel
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Photodiode Array Detection ◽  
Heat Condition ◽  
Stability Indicating ◽  
Dry Heat ◽  
Duloxetine Hydrochloride ◽  
Rp Hplc

Abstract This paper describes the development of a stability-indicating RP-HPLC method for duloxetine hydrochloride (DLX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was found to be susceptible to stress conditions of acid, base, oxidation, wet heat, dry heat, and photodegradation. The drug was found to be stable to the dry heat condition attempted. Successful separation of the drug from the degradation products formed under stress conditions was achieved on a Phenomenex C18 column (250 4.6 mm id, 5 µm particle size) using acetonitrilemethanol0.032 M ammonium acetate buffer (55 + 05 + 40, v/v/v) as the mobile phase at a flow rate of 1.0 mL/min at 40°C temperature. Quantification was achieved with photodiode array detection at 290 nm over the concentration range 0.25 µg/mL with mean recovery of 101.048 ± 0.53 for DLX by the RP-HPLC method. Statistical analysis proved the method is repeatable, specific, and accurate for estimation of DLX. Because the method could effectively separate the drug from its degradation products, it can be used as a stability-indicating method.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Guaifenesin and Dextromethorphan Impurities in Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Thummala V. Raghava Raju ◽  
Noru Anil Kumar ◽  
Seshadri Raja Kumar ◽  
Annarapu Malleswara Reddy ◽  
Nittala Someswara Rao ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
The Stability

A sensitive, stability-indicating gradient RP-HPLC method has been developed for the simultaneous estimation of impurities of Guaifenesin and Dextromethorphan in pharmaceutical formulations. Efficient chromatographic separation was achieved on a Sunfire C18, 250 × 4.6 mm, 5 µm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8 mL min−1 with column temperature of 50°C and detection wavelength at 224 nm. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for Guaifenesin, Dextromethorphan, and their impurities. Guaifenesin and Dextromethorphan formulation sample was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Guaifenesin was found stable and Dextromethorphan was found to degrade significantly in peroxide stress condition. The degradation products were well resolved from Guaifenesin, Dextromethorphan, and their impurities. The peak purity test results confirmed that the Guaifenesin and Dextromethorphan peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness.

scholarly journals Stability Indicating RP-HPLC for Quantification Mangiferin in Extract of Three Species Mango Leaves

2020 ◽  
Vol 8 (1) ◽  
pp. 15-20
Author(s):  
Yuni Retnaningtyas ◽  
Nia Kristiningrum ◽  
Hidayah Dwi Renggani ◽  
Indah Purnama Sary
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Mangifera Indica ◽  
Reversed Phase ◽  
Hplc Method ◽  
Complete Separation ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Mango Leaves ◽  
The Stability

The stability indication of Reversed Phase-High Performance Liquid Chromatography (RP-HPLC) method was validated for quantitative determination of mangiferin on three species mango leaves (Mangifera odorata Griff, Mangifera foetida Lour, and Mangifera indica L.). The samples were extracted by maseration method using methanol and concentrated using rotary evaporator. The method carried out on stationary phase a purospher RP-18 endcapped (25 cm × 4.6 mm i.d., 5 µm) column with a mobile phase consisting of methanol: phosphoric acid 0.1% (v/v) (31:69); flow rate:0.8 mL/min; solvent methanol, detection was carried out at 258 nm. The analytical  performace this measurement is good with the value of linearity (r2=0.998), precision (%RSD=0.649%), and accuration (10.67%). The forced degradation studies were carried out according to the International Conference on Harmonization (ICH) guidelines. The results indicating that the complete separation between degradation products and mangiferin peak occured. The degradation limit of mangiferin 5–20% (according to the guideline of ICH) except in basic condition (100%). The method was succesful applied to determine of the mangiferin in  pakel (Mangifera foetida), kweni (Mangifera indica) and kopyor (Mangifera odorata) extract. The mangiferin content was obtained are pakel (9.95%), kopyor (7.40%) and kweni (Mangifera odorata) (2.49%) respectively.

FORCED DEGRADATION STUDY OF POST-SHELF LIFE AND MARKETED TABLETS OF AMLODIPINE BY RP-HPLC

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 34-39
Author(s):  
M Puranik ◽  
◽  
P. G. Yeole ◽  
S. J. Wadher
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Point Of View ◽  
Forced Degradation ◽  
Dissolution Test ◽  
Amlodipine Besylate ◽  
Expiry Date ◽  
Rp Hplc ◽  
The Stability

The stability of pharmaceutical products plays an important role from the economical point of view. There are not many studies that report about the stability of drugs past their expiration dates. The objective of the current study was to determine tablet content and perform dissolution test of expired tablets of amlodipine besylate and tablets where expiry date has not exceeded and to develop simple, accurate, sensitive and stability indicating RP-HPLC method for the determination of per cent drug remained of Amlodipine besylate in the presence of its degradation products in bulk drug, expired tablets and tablets whose expiry date has not been exceeded. Drug was subjected to all stress conditions such as hydrolysis (acidic and alkaline), oxidation (3% H2O2 v/v), photolysis, thermal degradation and humidity study. Content determination was performed using spectrophotometric and RP-HPLC method; the per cent of dissolved substance from tablets during dissolution test was performed using spectrophotometric method and detection was made at 239 nm. All stressed samples were successfully analysed on C18 column using mobile phase phosphate buffer pH 3.5 (50mM): methanol: acetonitrile in the ratio of 30:60:10 v/v/v. A flow rate was maintained at 1.5 ml/min and detection was made at 240 nm. The proposed methods were validated with regard to linearity, sensitivity, and intermediate accuracy and precision. No discrepancies between the results of determination and the declared values range for all the analysed tablets were observed. The results of performed study might suggest that storage of analysed batches of tablets over time period exceeding the expiry date given by the manufacturer did not influence their contents.

TEM characterization of Au/Polysilicon interactions

1990 ◽  
Vol 48 (4) ◽  
pp. 650-651
Author(s):  
N. David Theodore ◽  
Leslie H. Allen ◽  
C. Barry Carter ◽  
James W. Mayer
Keyword(s):  
Solid Phase ◽  
Single Crystal Silicon ◽  
Chemical Vapor ◽  
Electrical Contacts ◽  
Silicon Substrates ◽  
Crystal Silicon ◽  
Transmission Electron ◽  
Polysilicon Films ◽  
The Stability

Metal/polysilicon investigations contribute to an understanding of issues relevant to the stability of electrical contacts in semiconductor devices. These investigations also contribute to an understanding of Si lateral solid-phase epitactic growth. Metals such as Au, Al and Ag form eutectics with Si. reactions in these metal/polysilicon systems lead to the formation of large-grain silicon. Of these systems, the Al/polysilicon system has been most extensively studied. In this study, the behavior upon thermal annealing of Au/polysilicon bilayers is investigated using cross-section transmission electron microscopy (XTEM). The unique feature of this system is that silicon grain-growth occurs at particularly low temperatures ∽300°C).Gold/polysilicon bilayers were fabricated on thermally oxidized single-crystal silicon substrates. Lowpressure chemical vapor deposition (LPCVD) at 620°C was used to obtain 100 to 400 nm polysilicon films. The surface of the polysilicon was cleaned with a buffered hydrofluoric acid solution. Gold was then thermally evaporated onto the samples.

The influence of the Stokes and Archimedes forces on the stability of a two-phase flow

2003 ◽  
Vol 3 ◽  
pp. 266-270
Author(s):  
B.H. Khudjuyerov ◽  
I.A. Chuliev
Keyword(s):  
Spectral Method ◽  
Stability Region ◽  
Gas Flow ◽  
Two Phase Flow ◽  
Solid Phase ◽  
Stability Characteristic ◽  
Phase Flow ◽  
Two Phase ◽  
The Stability

The problem of the stability of a two-phase flow is considered. The solution of the stability equations is performed by the spectral method using polynomials of Chebyshev. A decrease in the stability region gas flow with the addition of particles of the solid phase. The analysis influence on the stability characteristic of Stokes and Archimedes forces.

scholarly journals Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Lenalidomide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 35 (1) ◽  
pp. 140-149 ◽  
Author(s):  
Somana Siva Prasad ◽  
G. V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Stability Robustness ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Limit Of Quantitation ◽  
Successful Separation ◽  
Quality By Design Approach

In this study, a novel, simple and precise RP-HPLC method has been developed for the quantitative analysis of Lenalidomide (LLM) in pharmaceutical formulations using analytical quality by design approach. An X-bridge-C18 column (150 mm × 4.6 mm × 3.5 µ) with mobile phases containing a Potassium dihydrogen orthophosphate anhydrous buffer and methanol in the ratio of (90:10 v/v) and (35:65 v/v) are used for the estimation of LLM and its degradation products. The flow rate of 0.8 mL/min is maintained and all degradation studies are performed at 210 nm using photodiode array (PDA) detector. Method Validation is carried out according to International Council for Harmonisation (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful separation of LLM and its impurities in the pharmaceutical dosage formulations.

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