Immobilized Polysaccharide-Based Stationary Phases for Enantioseparation in Normal Versus Reversed Phase HPLC

2014 ◽  
Vol 78 (13-14) ◽  
pp. 909-915 ◽  
Author(s):  
Radim Geryk ◽  
Květa Kalíková ◽  
Jiří Vozka ◽  
Eva Tesařová
2012 ◽  
Vol 95 (6) ◽  
pp. 1639-1643 ◽  
Author(s):  
Michal Douša ◽  
Jiřiacute; Břicháč

Abstract A rapid HPLC method for the analytical resolution of cinacalcet enantiomers was developed. Four chiral columns (two amylose and two cellulose type) were evaluated in RP systems. Excellent enantioseparation with a resolution of more than 6 was achieved on Chiralpak AY (amylose 5-chloro-2-methylphenylcarbamate chiral stationary phase) using 10 mM triethylamine (pH 8.0)–acetonitrile (40 + 60, v/v) mobile phase. Validation of the HPLC method, including linearity, LOD, LOQ, precision, accuracy, and selectivity, was performed according to the International Conference on Harmonization guidelines. The method was successfully applied for the determination of (S)-cinacalcet in enantiopure active pharmaceutical ingredient (R)-cinacalcet.


2020 ◽  
pp. 81-88
Author(s):  
Viktor Ivanovich Deineka ◽  
Elena Yur'yevna Oleinits ◽  
Aleksandr Alekseyevich Pavlov ◽  
Andrey Yur'yevich Mikheev ◽  
Ol'ga Vladimirovna Shelepova ◽  
...  

The anthocyanin composition of some species of gooseberries with colored fruits was studied in comparison with anthocyanins of currant fruits from the collection of the Tsitsin Main Botanical garden. In fruits of currants Ribes nigrum var. sibiricum E. Wolf, R. nigrum L., R. americanum Mill., as well as in dark-colored fruits R. aureum Pursh., 3-glucosides and 3-rutinosides of cyanidin and delphinidin were found as major components in species-dependent ratios. It was found that in the fruits of gooseberry species Ribes oxyacanthoides L., Ribes missouriensis (Nutt.) Coville & Britton, Ribes rusticum Jancz. and Ribes cynosbati (L.) Mill. and in the fruits of one of the currants (R. alpinum L.) there is practically no biosynthesis of delphinidin derivatives, and 3-glucoside and 3-rutinoside of cyanidin are detected. Meanwhile, the biosynthesis of acylated by substituted cinnamic acids (mainly – p-coumaric acid) anthocyanins were found in the fruits of Ribes oxyacanthoides and Ribes cynosbati (about 10%), Ribes rusticum (about 20%). The inheritance of characteristic for the fruit of some species of gooseberry biosynthesis of acylated mainly p-coumaric acid, was installed in the fruits of jostaberry - Ribes x nidigrolaria Rud. Bauer & A. Bauer (about 10%). The species composition of anthocyanins was established using traditional reversed-phase HPLC in gradient elution mode using diode-array and mass spectrometric detection options. In addition, a method for the separation of anthocyanins of the same objects in the isocratic mode under hydrophilic interaction chromatography on diol stationary phases, allowing the use of simpler equipment. The variants of sample preparation of extract samples for the subsequent HPLC determination of anthocyanins by two different methods to avoid the appearance of artifacts are proposed.


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