Vulcanized rubber - Determination of free sulfur by gas chromatography (GC) and high performance liquid chromatography (HPLC)

2019 ◽  
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Vulcanized Rubber ◽  
Free Sulfur

Determination of Impurities in Perampanel Bulk Drugs by High-Performance Liquid Chromatography and Gas Chromatography

2020 ◽  
Vol 16 ◽  
Author(s):  
Yun-Yan Xia ◽  
Qiao-Gen Zou ◽  
Yu-Fei Yang ◽  
Qian Sun ◽  
Cheng-Qun Han
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Quantitative Detection ◽  
Dihydrogen Phosphate ◽  
Phosphate Solution ◽  
Related Impurities ◽  
Bulk Drug

Background: High-performance liquid chromatography (HPLC) method has been used to detect related impurities of perampanel. However, the detection of impurities is incomplete, and the limits of quantification and detection are high. A sensitive, reliable method is in badly to be developed and applied for impurity detection of perampanel bulk drug. Objective: Methodologies utilising HPLC and gas chromatography (GC) were established and validated for quantitative determination of perampanel and its related impurities (a total of 10 impurities including 2 genotoxic impurities). Methods: The separation was achieved on a Dikma Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.01 mol/L potassium dihydrogen phosphate solution (A) and acetonitrile (B) in gradient elution mode. The compound 2-bromopropane was determined on an Agilent DB-624 column (0.32 mm × 30 m, 1.8 μm) by electron capture detector (μ-ECD) with split injection ratio of 1:5 and proper gradient temperature program. Result: Both HPLC and GC methods were established and validated to be sensitive, accurate and robust according to International Council for Harmonization (ICH) guidelines. The methods developed were linear in the selected concentration range (R 2≥0.9944). The average recovery of all impurities was between 92.6% and 103.3%. The possible production mechanism of impurities during the synthesis and degradation processes of perampanel bulk drug was also discussed. Five impurities were analyzed by liquid chromatography–mass spectrometry (LC-MS). Moreover, two of them were simultaneously characterized by LC-MS, IR and NMR. Conclusion: The HPLC and GC methods were developed and optimized, which could be applied for quantitative detection of the impurities, and further stability study of perampanel.

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.

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