Qualitative and Quantitative Chemometry as Stability-Indicating Methods for Determination of Dantrolene Sodium and Paracetamol

2017 ◽  
Vol 14 (1) ◽  
Author(s):  
Ali M. Yehia ◽  
Iman Sami ◽  
Safa'a M. Riad ◽  
Yasser S. El-Saharty
Keyword(s):  
Dantrolene Sodium ◽  
Stability Indicating ◽  
Qualitative And Quantitative

Comparison of standardised lymphoscintigraphic function test and high resolution sonography of the lymphoedema of legs

Phlebologie ◽  
2008 ◽  
Vol 37 (05) ◽  
pp. 247-252 ◽  
Author(s):  
V. S. Brauer ◽  
W. J. Brauer
Keyword(s):  
Lower Leg ◽  
Clinical Findings ◽  
Lower Limbs ◽  
Fatty Tissue ◽  
Qualitative And Quantitative ◽  
Function Test ◽  
Unreliable Method ◽  
Negative Conclusion ◽  
Fine Disperse

SummaryPurpose: Comparison of qualitative and quantitative sonography with the lymphoscintigraphic function test and clinical findings in legs. Patients, methods: In 33 patients a lymphoscintigraphic function test of legs combined with measurement of lymph node uptake was performed and subsequently compared with sonography. Sonographic criteria were: Thickness of cutis, thickness of subcutanean fatty tissue and presence of liquid structures or fine disperse tissue structure of lower limbs, foots and toes. Results: In 51 legs uptake values lie in the pathologic area, in four legs in the grey area and in ten legs in the normal area. The cutis thickness in the lower leg shows no significant correlation with the uptake. The determination of the thickness of the subcutanean fatty tissue of the lower leg and of the cutis thickness of the feet turned out to be an unreliable method. In 47% of the medial lower legs and in 57% of the lateral lower legs with clinical lymphoedema sonography is falsely negative. Conclusion: Early lymphoedema is only detectable with the lymphoscintigraphic function test. In the case of clinical lymphoedema clinical examination is more reliable than sonography.

Development of Validated Stability Indicating HPTLC Method for Assay of Ozagrel and its Pharmaceutical Formulations

2018 ◽  
pp. 36-48 ◽  
Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production ◽  
Hptlc Method

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.

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.  

The Comparative Study of Equisetum pratense, E. sylvaticum, E. telmateia: Accumulation of Silicon, Antioxidant and Antimicrobial Screening

2019 ◽  
Vol 70 (7) ◽  
pp. 2519-2523
Author(s):  
Denisa Batir Marin ◽  
Oana Cioanca ◽  
Mihai Apostu ◽  
Cristina Gabriela Tuchilus ◽  
Cornelia Mircea ◽  
...  
Keyword(s):  
Antimicrobial Activity ◽  
Methanol Extract ◽  
Previous Treatment ◽  
Total Phenolic ◽  
Quantitative Chemical Analysis ◽  
Qualitative And Quantitative ◽  
Antioxidant And Antimicrobial Activity ◽  
The Comparative Study

The objective of the current study is represented by the determination of silica and a phytochemical screening of phenolic derivates of some Equisetum species. The antioxidant and antimicrobial activity for Equisetum pratense Ehrh.,, Equisetum sylvaticum L. and Equisetum telmateia Ehrh. (sin. Equisetum maximum Lam.) were also investigated. The concentration of silicon (Si) in plants was determined by the spectrophotometric method using previous treatment with NaOH 50% both for the stem and the nodal branches [1]. Results obtained varied from 95.12 to 162.10 SiO2 mg/g dry plant which represents 4.44% to 7.58% Si/100g dry sample. Two types of total extracts were obtained using different solvents and were subjected to qualitative and quantitative chemical analysis considering total phenolic content [2]. The highest concentration of investigated compounds was found in the methanolic extract, E. sylvaticum, 196.5mg/g dry sample. Antioxidant activity was monitored spectrophotometrically and expressed in terms of IC50 (�g/mL) [3]. Values gathered ranged from 261.7 to 429.5 �g/mL. The highest capacity to neutralized DPPH radicals was found in E. sylvaticum. In vitro antimicrobial activity was determined using difusimetric method [4]. Testing was performed on four microorganisms: three strains of bacteria and one species of fungi. Different effects were noticed against the bacteria, furthermore the methanol extract appeared to be most efficient. All extracts showed significand antimicrobial activity against Staphylococcus aureus (ATCC 25923) and Candida albicans (ATCC 90028) and weak to no activity against Pseudomonas aeruginosa (ATCC 27853) and Escherichia coli (ATCC 25922).

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.

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