scholarly journals RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini
Keyword(s):  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Column Temperature ◽  
Layer Chromatography

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100-600 and 4-24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1-10 and 0.32-3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.

scholarly journals High Performance Liquid Chromatography (HPLC) Stability Indicating Method for the Determination of Bromazepam Via its Copper (II) Chelates

2017 ◽  
Vol 4 (1) ◽  
pp. 32-42 ◽  
Author(s):  
Assefa Takele ◽  
Abdel-Maaboud I. Mohamed Attaya ◽  
Ariaya Hymete ◽  
Melisew Tadele Alula
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Azomethine Nitrogen ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method

Introduction: Bromazepam is hydrolyzed in acidic aqueous solution leading to a series of degradation products. The rate of acidic hydrolysis is believed to be dependent on the state of protonation of the pyridyl and azomethine nitrogen atoms. Stability test is important in pharmaceutical industry to provide evidence on how the quality of an active substance or pharmaceutical product varies with time under the influence of a variety of environmental factors. Objective: The aim of the study was to develop a simple stability indicating method for the determination of bromazepam. Method: Bromazepam solution was prepared and forced degradation of bromazepam was performed under acid hydrolysis using sulphuric acid. High performance liquid chromatography determination of pure and degraded bromazepam and bromazepam-copper (II) complex was performed using reversed phase octyl C-8 column under isocratic conditions and the chromatographic conditions were set as follows; the flow rate of the mobile phase was 1.5 mL/min; injection volume was 10 μL, column temperature was 30oC and the detector wavelength being 309 nm. Results: Bromazepam, its degradation product and bromazepam chelated with copper (II) were determined using the developed mobile phase with flow rate of 1.5 mL/min. Good separation with sharp peak, minimum tailing and retention time repeatability was obtained. The rate order, rate constant and half-life of degradation were also determined, and it was observed that the degradation reaction follows the first order kinetics. Conclusion: Chromatographic separation of bromazepam chelated with copper (II) was achieved and the method can be further used in drug manufacturing quality control.

Quantitative Determination of Vitamin E Isomers using Gas Chromatography, High Performance Liquid Chromatography and High Performance Thin Layer Chromatography

2017 ◽  
Vol 54 (3) ◽  
pp. 294
Author(s):  
Hari Ramakrishnan K. ◽  
Janaky Ranjithkumar
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Vitamin E ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Highly Sensitive ◽  
Layer Chromatography

Vitamin E, the fat soluble vitamin is present naturally in some foods and added in food supplements, nutraceuticals etc due to its vital biological function as an antioxidant. Various methods are available for the analysis of vitamin E. Especially High Performance Liquid Chromatography (HPLC) and Gas Chromatography (GC) are exclusively used for the quantitative evaluation of vitamin E, which has also identified the four different isomeric forms of this vitamin. The rate of losses of this vitamin during food processing and analysis, in addition to their transient dynamics, presents complexities in developing a highly sensitive procedure for their separations. Though effective, HPLC instrument is expensive and comparatively cumbersome. In this prospective, the study was to evaluate the usefulness of High Performance Thin Layer Chromatography (HPTLC) in the analysis of vitamin E. There are methods available using Thin Layer Chromatography for its analysis, but they are not sensitive enough to identify the isomeric forms of vitamin E. In this HPTLC method, the different isomeric forms of vitamin E - α, β, γ and δ were identified. This technique shall be considered as an alternative to the other methods such as HPLC and GC.

Sign in / Sign up

Export Citation Format

Share Document