Cross validation of capillary electrophoresis and high-performance liquid chromatography for cefotaxime and related impurities

Background: Many antibiotics were widely used as medication based on their distinctive features. Among them, sulphonamides were commonly used, however their recalcitrant nature makes them difficult to dispose. Hence, their interaction with environment and analytic technique requires considerable attention globally. Objective: Therefore, this review aimed to provide detailed discussion about environmental as well as human health behaviour and analytic techniques corresponding to sulphonamides. Methods: Various results and discussion were extracted from technical journals and books published by different researchers from all over the world. The cited bibliographic references were intentionally investigated in order to extract relevant information related to proposed work. Results: In this review, the determination techniques such as UV-spectroscopy, Enthalpimetry, Immunosensor, Chromatography, Chemiluminescence, Photoinduced fluorometric determination, Capillary electrophoresis for sulphonamide determination were discussed in detail. Among them, High performance liquid chromatography (HPLC) and UV-spectroscopy was effective and extensively used for screening sulphonamide. Conclusion: Knowing the quantification and behaviour of sulphonamide in aqueous solution is mandatory to opt the suitable wastewater treatment required. Hence, choosing appropriate high precision and feasible screening techniques is necessary, which can be attained with this review.

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

Current Pharmaceutical Analysis ◽

10.2174/1573412916999200513105657 ◽

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.

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