Rapid Thin-Layer-Chromatographic Methods for the Determination of Microbiological Degradation Products of Deoxynivalenol

1997 ◽  
Vol 25 (3) ◽  
pp. 361-362
Author(s):  
N. Ellend ◽  
E. M. Horvath ◽  
J. Binder ◽  
R. Braun ◽  
R. Krska
Keyword(s):  
Thin Layer ◽  
Degradation Products ◽  
Chromatographic Methods

Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pharmaceutical Analysis ◽  
High Performance ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Accuracy And Precision ◽  
Post Marketing ◽  
Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

Collaborative Study of a Method for the Determination of Ochratoxin A in Green Coffee

1975 ◽  
Vol 58 (2) ◽  
pp. 258-262 ◽  
Author(s):  
Colette P Levi
Keyword(s):  
Thin Layer ◽  
Ochratoxin A ◽  
Collaborative Study ◽  
Green Coffee ◽  
Average Recovery ◽  
Semiquantitative Determination ◽  
Chromatographic Methods ◽  
Green Coffee Beans ◽  
Coffee Beans

Abstract A method for the semiquantitative determination of ochratoxin A in green coffee has been studied collaboratively by 11 laboratories. The average recovery for the 7 samples spiked at 3 levels of ochratoxin A was 69.1%, ranging from 60.5 to 85.6%. This is comparable to other visual thin layer chromatographic methods of mycotoxin detection. The method has been adopted as official first action for the determination of ochratoxin A in green coffee beans.

scholarly journals Validated Stability Indicating HPTLC Method for the Determination of Dutasteride in Pharmaceutical Dosage Forms

2011 ◽  
Vol 2011 ◽  
pp. 1-5 ◽  
Author(s):  
Dipti B. Patel ◽  
Natubhai J. Patel ◽  
Sejal K. Patel ◽  
Paresh U. Patel
Keyword(s):  
Thin Layer ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Wet Heat ◽  
Pure Drug

This paper describes simple, sensitive, precise, specific, and stability-indicating high-performance thin-layer chromatographic method for the determination of dutasteride (DUTA) in bulk and tablet formulation. Validation was carried out in compliance with International Conference on Harmonization guidelines. The thin-layer chromatographic method employed aluminium plates precoated with silica gel G60F254 as stationary phase. The solvent system consisted of toluene/methanol/triethylamine (9 : 2 : 1, v/v/v). This solvent system was found to give compact spots for dutasteride with value 0.71 ± 0.01. Densitometric analysis of DUTA was carried out in the absorbance mode at 274 nm. Linear regression analysis showed good linearity () with respect to peak area in the concentration range of 200–3000 ng per spot. The method was validated for precision, accuracy, specificity, and robustness. Pure drug was subjected to acid and alkali hydrolysis, oxidation, photo degradation, dry heat and wet heat treatment. The drug underwent degradation under acidic, basic, oxidative, and wet heat conditions. The degraded products were well separated from the pure drug. Statistical analysis proved that the method is reproducible and selective for estimation of DUTA in bulk and tablets. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

Development and Validation of Two Robust Stability-Indicating Chromatographic Methods for Determination of Metolazone in Drug Substance and Pharmaceutical Dosage Form in the Presence of Its Degradation Products and Characterization of Main Degradation Products Based on LC-MS

2019 ◽  
Vol 58 (3) ◽  
pp. 251-261
Author(s):  
Hala E Zaazaa ◽  
Rasha Abdel-Ghany ◽  
M Abdelkawy ◽  
Mahmoud Sayed
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Drug Substance ◽  
Design Parameters ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Chromatographic Methods ◽  
Hptlc Method

Abstract Two robust and selective stability-indicating chromatographic methods were developed and validated for the determination of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The HPLC method employed a Kromasil C18 (250 × 4.6,5 μm) column and a mobile phase of acetonitrile: 0.2% orthophosphoric acid (32:68 v/v) at a flow rate 2 mL/min and detection at 238 nm. The separation was performed in HPLC isocratic mode. The robustness of the suggested method was assessed using the Plackett–Burman design, parameters affecting system suitability were established and non-significant intervals for the significant parameters were considered. The HPTLC method employed Nano-SIL-20 UV254 HPTLC plates as adsorbent, ethyl acetate: toluene: acetic acid solution (4:4:0.5, v/v/v), as a developing solvent system and densitometric detection at 238 nm. Metolazone was exposed to different stress conditions, including acid and alkaline hydrolysis and oxidative and photolytic degradation. The main degradation products obtained have been characterized and interpreted based on LC-MS. The linearity of the suggested methods was proved in the concentration range of 20–75 μg/mL for the HPLC method and 100–900 ng/spot for the HPTLC method. The suggested methods were validated according to international conference on harmonization guidelines. These methods were successfully dedicated for the estimation of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The results of the suggested methods were evaluated and compared statistically with results obtained by an official method without finding any significant difference.

Development of two high-performance thin-layer chromatographic methods for the determination of irbesartan in tablets and plasma

2015 ◽  
Vol 28 (1) ◽  
pp. 83-89 ◽  
Author(s):  
Samiha El-Rahman Hussein ◽  
Hanaa El-Wadood ◽  
Mohamed Abou-Elwafa Abdallah ◽  
Ahmed El-Hamid Khorshed
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Chromatographic Methods

scholarly journals Validated Stability – Indicating Methods for Determination of Sofosbuvir by UPLC and HPTLC in Pure Form and Tablet Dosage Forms

2019 ◽  
pp. 1-13
Author(s):  
Sawsan A. Abdel-Razeq ◽  
Zeinab Adel Nasr ◽  
Noha S. Said
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
High Performance ◽  
Good Accuracy ◽  
Degradation Products ◽  
Dosage Forms ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of sofosbuvir in presence of its degradation products. Study Design: Ultra high performance liquid chromatography (UPLC), High performance thin layer chromatography (HPTLC) are developed for determination of sofosbuvir in presence of its degradation products, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, between August 2018 and March 2019. Methodology: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of Sofosbuvir in presence of its degradation products. The first method was an Ultra Performance Liquid Chromatography (UPLC) method, in which efficient separation was carried out on phenomenex kinetex 2.6 μm C18 100 A column using a mobile phase consisting of filtered and degassed mixture of 0.1% ortho-phosphoric acid in water and methanol with the ratio of (40:60% v/v) adjusted to pH 3.5, at a flow rate of 1 mL min-1 and UV detection at 260 nm at ambient temperature. The second method is a high performance- thin layer chromatographic one (HPTLC) in which chromatographic separation was performed on silica gel 60 F254 plates, with methanol – chloroform – ammonia (2.5: 6: 1.5 % v/v/v) as a developing system followed by densitometric determination at 261 nm. Sofosbuvir was subjected to stress conditions including alkaline, acidic and oxidative degradation. Results: Beer’s law was obeyed over the range of 1-20 μg mL–1 for UPLC and 2-12 μg / spot for HPTC with good accuracy and precision using the two procedures, respectively. Results obtained was statistically analysed and found to be in accordance with those given by the reported method. Conclusion: The proposed methods were successfully applied for the determination of sofosbuvir in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Validated Stability Indicating Chromatographic Methods for Quantification of Imidocarb Dipropionate; Application for the Determination of Its Residues in Bovine Meat and Milk Samples

2020 ◽  
Vol 103 (4) ◽  
pp. 980-988
Author(s):  
Ghada AbdElHamid Sedik ◽  
Doha Mohamed Naguib ◽  
Fahima Morsy ◽  
Hala Elsayed Zaazaa
Keyword(s):  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Milk Samples ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Imidocarb Dipropionate ◽  
Tlc Plates

Abstract Background Imidocarb dipropionate (IMD) is an immunomodulator agent commonly used for treatment of anaplasmosis in cattle. Objective Thus, two sensitive, specific, and precise stability-indicating chromatographic methods have been developed, optimized, and validated for its determination in presence of its acid, alkaline, and oxidative stressed degradation products. Method The first method is based on separation of IMD and its forced induced degradation products on reversed phase cyano column using isocratic elution system consisted of sodium acetate buffer–methanol–acetonitrile (55: 30:15, v/v/v), pH 4.6 at a flow rate of 1.2 mL/min, and UV detection at 254 nm. The second method utilized TLC combined with densitometric determination of the separated bands at 254 nm. The separation was achieved using silica gel 60 F254 TLC plates with a mixture of ethyl acetate–methanol–ammonia–water (8.5:1:0.5:0.2, v/v/v/v) as a developing system. Results HPLC analysis was applied in range of 0.25–40 µg/mL with LOD of 0.073 µg/mL. While densitometric measurements showed linearity in the range of 0.1–1.8 µg/band with LOD of 0.02 µg/band. Conclusions The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of IMD in its commercial veterinary formulations with good recoveries. Furthermore, the proposed HPLC method was extended to the determination of IMD residues in bovine meat and milk samples Highlights Bovine meat, HPLC, Imidocarb dipropionate, Milk, TLC.

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