Occurrence of tertiary branched tetraamines in two aquatic plants

2000 ◽  
Vol 78 (2) ◽  
pp. 266-269
Author(s):  
Koei Hamana ◽  
Masaru Niitsu ◽  
Keijiro Samejima
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Aquatic Plants ◽  
High Performance ◽  
Aquatic Plant ◽  
Pistia Stratiotes ◽  
Whole Plants ◽  
Potamogeton Distinctus

Four aquatic plants were tested for the occurrence of unusual polyamines by high performance liquid chromatography and gas chromatography. The whole plants ubiquitously contained norspermidine, homospermidine, norspermine, and thermospermine in addition to usual polyamines such as diaminopropane, putrescine, spermidine, and spermine. Pistia stratiotes L. and Potamogeton distinctus A. Bennett contained aminopropylhomospermidine. Caldopentamine was detected in the former plant. Homospermine was found in Ranuculus aquatilis L. Two tertiary branched tetraamines, N4-aminopropylnorspermidine and N4-aminopropylspermidine, were detected in Potamogeton distinctus and Sagittaria trifolia L.Key words: aquatic plant, polyamine, tertiary branched tetraamine.

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.

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