Separation of fluorescent 1,N6 ethenoderivatives of diadenosine polyphosphates and their enzymatic degradation products by reversed-phase high-performance liquid chromatography

1991 ◽  
Vol 32 (7-8) ◽  
pp. 350-356 ◽  
Author(s):  
A. Ramos ◽  
M. Guerra ◽  
P. Rotllán
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Enzymatic Degradation ◽  
Degradation Products ◽  
Reversed Phase ◽  
Diadenosine Polyphosphates

Identification of tuliposide G, a novel glucoside ester-type tuliposide, and its distribution in tulip

2020 ◽  
Vol 75 (3-4) ◽  
pp. 75-86
Author(s):  
Taiji Nomura ◽  
Yasuo Kato
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Secondary Metabolites ◽  
High Performance ◽  
Enzymatic Degradation ◽  
Degradation Products ◽  
Tulipa Gesneriana ◽  
Tissue Extracts ◽  
Spectroscopic Analyses ◽  
Chemotaxonomic Marker

AbstractTuliposides (Pos) are major defensive secondary metabolites in tulip (genus Tulipa), having 4-hydroxy-2-methylenebutanoyl and/or (3S)-3,4-dihydroxy-2-methylenebutanoyl groups at the C-1 and/or C-6 positions of d-glucose. The acyl group at the C-6 position is converted to antimicrobial lactones, tulipalins, by tuliposide-converting enzymes (TCEs). In the course of a survey of tulip tissue extracts to identify novel Pos, we found a minute high-performance liquid chromatography peak that disappeared following the action of a TCE, and whose retention time differed from those of known Pos. Spectroscopic analyses of the purified compound, as well as its enzymatic degradation products, revealed its structure as 5″-O-(6-O-(4′-hydroxy-2′-methylenebutanoyl))-β-d-glucopyranosyl-(2″R)-2″-hydroxymethyl-4″-butyrolactone, which is a novel glucoside ester-type Pos. We gave this compound the trivial name ‘tuliposide G’ (PosG). PosG accumulated in bulbs, at markedly lower levels than 6-PosA (the major Pos in bulbs), but was not found in any other tissues. Quantification of PosG in bulbs of 52 types of tulip, including 30 cultivars (Tulipa gesneriana) and 22 wild Tulipa spp., resulted in the detection of PosG in 28 cultivars, while PosG was present only in three wild species belonging to the subgenus Tulipa, the same subgenus to which tulip cultivars belong, suggesting the potential usefulness of PosG as a chemotaxonomic marker in tulip.

Development and Validation of a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) Method for Identification, Assay and Estimation of Related Substances of Ivermectin in Bulk Drug Batches of Ivermectin Drug Substance

2021 ◽  
Author(s):  
Daoli Zhao ◽  
Rasangi M Wimalasinghe ◽  
Lin Wang ◽  
Abu M Rustum
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Substance ◽  
Related Impurities ◽  
Rp Hplc ◽  
Bulk Drug

Abstract A reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for the identification and assay of Ivermectin, including the identification and estimation of its process-related impurities and degradation products in bulk drug substance of Ivermectin. Analytes were separated on a HALO C18 column (100 mm × 4.6 mm I.D., 2.7 μm particle size) maintained at 40 °C (column temperature) with gradient elution. All analytes of interests were adequately separated within 25 min. All degradation products, process-related impurities and assay were monitored by ultraviolet detection at 254 nm. The new HPLC method described here successfully separated an isomer peak of the active pharmaceutical ingredient (API) from the major API peak. This newly separated isomer peak is around 1.2 to 1.5% (peak area) in typical API samples, and coelutes with the major API peak by all current HPLC methods. Quantitation limit of the HPLC method is 0.1% of target analytical concentration (~1.0 μg/mL). This method has been demonstrated to be accurate, robust, significantly higher degree of selectivity compared to the HPLC methods of Ivermectin drug substance reported in the literature and in the compendial HPLC methods prescribed in the current USA and European Pharmacopeia.

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