scholarly journals A stability-indicating LC–MS/MS method for zidovudine: Identification, characterization and toxicity prediction of two major acid degradation products

2017 ◽  
Vol 7 (4) ◽  
pp. 231-236 ◽  
Author(s):  
Prashant S. Devrukhakar ◽  
M. Shiva Shankar ◽  
G. Shankar ◽  
R. Srinivas
Keyword(s):  
Degradation Products ◽  
Toxicity Prediction ◽  
Stability Indicating ◽  
Acid Degradation ◽  
Major Acid

Stability-Indicating Determination of Rebamipide in the Presence of its Acid Degradation Products

2014 ◽  
Vol 97 (1) ◽  
pp. 78-85 ◽  
Author(s):  
Samah S Abbas ◽  
Hala E Zaazaa ◽  
Hebat Allah M Essam ◽  
Mohammed G El-Bardicy
Keyword(s):  
Degradation Products ◽  
Complete Separation ◽  
Peak Amplitude ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Rp Hplc ◽  
Absorbance Difference

Abstract Four sensitive and precise stability-indicating methods for the determination of rebamipide (REB) in the presence of its acid-degradation products and ina pharmaceutical formulation were developed and validated. Method A used the first derivative of the ratio spectra (1DD) spectrophotometric method by measuring the peak amplitude at 249.4 nm (maximum) and at 259 nm (minimum), and at the total peak amplitude (from 249.4 to 259 nm, 1DD249.4 + 259 nm) in the range of 2–14 μg/mL. This method yielded mean recoveries of 99.87 ± 0.83, 100.04 ± 0.75, and 100.28 ± 1.11%, respectively. Method B is a dual wavelength method, which allows the determination of REB in presence of its acid-degradation products by measuring the absorbance difference between 254 and 269 nm within a linearity range of 5–65 μg/mL; it showed a mean recovery of 99.84 ± 1.06. Method C is a TLC-densitometric procedure in which REB was separated from its degradation products using a developing solution of methanol–chloroform–ammonia (8.5 + 1.5 + 0.5, v/v/v). The quantitative evaluation of REB at 329 nm was linear over the concentration range of 0.50–4.5 μg/band, with a mean recovery of 99.49 ± 0.99% even in the presence of up to 90% degradation products. Method D is an RP-HPLC procedure. It provided the complete separation of REB from its degradation products on an XterraTM C18 column using phosphate buffer (pH 6, 0.01 M)–methanol (1 + 1, v/v) as the mobile phase (UV detection at 254 nm). Recovery was 99.28 ± 0.78% within the range of 10–190 μg/mL. The selectivity of the proposed methods was checked using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of REBin pharmaceutical dosage forms without interference from other dosage form excipients.

Stability-Indicating Spectrofluorometric Method for the Determination of Some Cephalosporin Drugs via Their Degradation Products

2015 ◽  
Vol 98 (2) ◽  
pp. 361-370 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Excitation Wavelength ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
Accuracy And Precision ◽  
Spectrofluorometric Method ◽  
Good Agreement

Abstract A stability-indicating spectrofluorometric method was investigated for the determination of three cephalosporin drugs, namely, cefpodoxime proxetil (CPD), cefixime trihydrate (CFX), and cefepime hydrochloride (CPM), via their acid and alkali degradation products. The three drugs were determined via their acid degradation at 432, 422, and 435 nm using an excitation wavelength of 310, 330, and 307 nm for CPD, CFX, and CPM determination, respectively, and via their alkali degradation at 407, 411, and 405 nm using an excitation wavelength of 310, 305, and 297 nm for CPD, CFX, and CPM determination, respectively. Linearity was achieved in the ranges of 0.35–3.50,0.4–4.0, and 0.3–3.0 μg/mL for the acid degradation products of CPD, CFX, and CPM, respectively, and in ranges of 0.05–0.5, 0.1–1.0, and 0.08–0.80 μg/mL for the alkali degradation products of CPD, CFX, and CPM, respectively. The method was validated for various parameters according to International Conference on Harmonization guidelines. The method was successfullyapplied for the determination of these cephalosporindrugs in pharmaceutical dosage forms with good accuracy and precision. The results obtained by the proposed spectrofluorometric method were compared with good agreement to the official HPLC method.

scholarly journals STABILITY-INDICATING METHODS FOR THE DERTERMINATION OF GEMIFLOXACIN IN PRESENCE OF ITS ACID DEGRADATION PRODUCT(S)

2015 ◽  
Vol 11 (6) ◽  
pp. 3698-3708
Author(s):  
Fatma Alamin ◽  
Ezzat Abdel Moety ◽  
Amr Badawey ◽  
Heba Hefne
Keyword(s):  
Degradation Products ◽  
Zero Crossing ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Wide Range ◽  
Intact Drug ◽  
Minimal Data ◽  
The Difference

Brilliant, valid and simple five UV spectrophotometric stability indicating techniques are adopted for the determination of Gemifloxacin (GEM) in presence of its acid degradation products over a concentration range of 2-12 μg mL-1. The first method is an application of the first derivative (1D) spectrophotometry, that allows the determination of GEM without interference of its acid degradation products at zero crossing wavelength (254.6 nm). The second method depends on the first-derivative of the ratio spectra spectrophotometry (1DD) for determination of GEM in presence of its acid degradation products at a maximum of 273.0 nm and a minimum of 284.0 nm, While the third dual wavelength method offers a superior stability indicating procedures for the determination of GEM in the zero order spectra at the wavelength pair of 271.8 nm and 325.0 nm. The fourth method is the ratio difference one, with the advantages of minimal data processing and wide range of application. It is applied for the analysis of intact drug in presence of its acid degradation products by measuring the difference in the peak amplitude at the ratio spectra at 355.0 nm and 270.0 nm. The last method is based on the quantification of GEM through the bivariate calibration at 255.0 nm and 277.0 nm by adopting simple mathematic algorithm that provides simplicity and rapidity.

Stability-Indicating Methods for the Determination of Erdosteine in the Presence of its Acid Degradation Products

2014 ◽  
Vol 97 (1) ◽  
pp. 86-93 ◽  
Author(s):  
Nadia M Moustafa ◽  
Amr M Badawey ◽  
Nesrine T Lamie ◽  
Abd El-Aziz B Abd El-Aleem
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Validity Of Results ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Percentage Recovery ◽  
The Mean

Abstract Four accurate, sensitive, and reproducible stability-indicating methods for the determination of erdosteine in the presence of its acid degradation products are presented. The first method involves processing the spectra by using a first-derivative method at 229 nm in a concentration range of 10–70 μg/mL. The mean percentage recovery was 100.43 ± 0.977. The second method is based on ratio-spectra first derivative spectrophotometry at 227.4 and 255 nm over a concentration range of 10–70 μg/mL. The mean percentage recovery was 99.65 ± 1.122% and 100.02 ± 1.306% at 227.4 and 255 nm, respectively. The third method utilizes quantitative densitometric evaluation of the TLC of erdosteine in the presence of its acid degradation products, and uses methanol–chloroform–ammonia (7 + 3 + 0.01, v/v/v) asthe mobile phase. TLC chromatograms were scanned at235 nm. This method analyzes erdosteine in a concentration range of 2.4–5.6 μg/spot, with a mean percentage recovery of 100.03 ± 1.015%. The fourth method is HPLC for the simultaneousdetermination of erdosteine in the presence of its acid degradation products. The mobile phase consists of water–methanol (65 + 35, v/v). The standard curve of erdosteine showed good linearity overa concentration range of 10–80 μg/mL,with a mean percentage recovery of 99.90 ± 1.207%. These methods were successfully applied to the determination of erdosteine in bulk powder, laboratory-prepared mixtures containing different percentages of the degradation products, and pharmaceutical dosage forms. The validity of results was assessed by applying the standard addition technique. The results obtained agreed statistically with those obtained by a reported method, showing no significant differences with respect to accuracy and precision.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

2019 ◽  
Vol 15 (3) ◽  
pp. 273-279
Author(s):  
Shweta G. Rangari ◽  
Nishikant A. Raut ◽  
Pradip W. Dhore
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Analysis Data ◽  
Peak Height ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

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