Chromatographic behavior of a new hybrid type RP material containing silica bonded 1,3-alternate 25,27-bis-[cyanopropyloxy]-26,28-bis-[3-propyloxy]-calix[4]arene

A novel 1,3-alternate 25,27-bis-[cyanopropyloxy]-26,28-bis-[3-propyloxy]-calix[4]arene-bonded silica gel stationary phase (CalixPrCN) was prepared and its structure was confirmed by ATR-FTIR spectroscopy and elemental analysis. The CalixPrCN phase was characterized in terms of its surface coverage,...

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Bibliographic Details
Published in:Journal of separation science 2010-10, Vol.33 (19), p.2956-2964
Main Authors: Sliwka-Kaszynska, Magdalena, Lepicka, Kamila, Slebioda, Marek
Format: Article
Language:English
Subjects:
Acetonitrile
Calixarene stationary phase
Calixarenes
Column characterization
Columns (structural)
Drugs
Materials selection
Retention mechanism
Selectivity
Separation
Silica gel
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Summary:A novel 1,3-alternate 25,27-bis-[cyanopropyloxy]-26,28-bis-[3-propyloxy]-calix[4]arene-bonded silica gel stationary phase (CalixPrCN) was prepared and its structure was confirmed by ATR-FTIR spectroscopy and elemental analysis. The CalixPrCN phase was characterized in terms of its surface coverage, hydrophobic selectivity, aromatic selectivity, shape selectivity, hydrogen bonding capacity, residue metal content, and silanol activity based on Tanaka, Lindner, and SMR 870 test protocols. The effect of the acetonitrile content on the retention and selectivity of the selected neutral, basic, and acidic solutes was studied. The neutral and acidic analytes exhibited classical RP behavior, in which retention time decreases with increasing acetonitrile content. In contrast, basic analytes showed an increase in retention at low and high percentages of acetonitrile, forming "U-shaped" retention profiles. The new calixarene phase was compared with previously reported 1,3-alternate 25,27-bis-[propyloxy]-26,28-bis-[3-propyloxy]-calix[4]arene stationary phase and commercial cyanopropyl column. The results indicate that the CalixPrCN stationary phase behaves like RP packing; however, inclusion complex formation, dipole-dipole, and π-π interactions seem to be involved in the separation process. The selectivity of this phase was demonstrated in separation of polynuclear aromatic hydrocarbons, non-steroidal anti-inflammatory drugs, and sulfonamides as analytes.
ISSN:1615-9306
1615-9314
1615-9314
DOI:10.1002/jssc.201000263