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  • Investigation of novel immobilized 3-(perfluoroalkanoyl)-(1R)-camphorate nickel complexes in enantioselective complexation gas chromatography.

Investigation of novel immobilized 3-(perfluoroalkanoyl)-(1R)-camphorate nickel complexes in enantioselective complexation gas chromatography.

Journal of chromatography. A (2012-08-23)
Skrollan Stockinger, Markus J Spallek, Oliver Trapp
ABSTRACT

Novel 3-(perfluoroalkanoyl)-(1R)-camphorate nickel complexes immobilized to poly(dimethylsiloxane) phases are presented. Immobilized 3-(perfluoroalkanoyl)-(1R)-camphorate nickel complexes with a trifluoromethyl (CF(3); nickel(II)-bis[(1R,4S)-3-trifluoromethanoyl-10-propylenoxycamphor]-polysiloxane Ni(tfpc)(2)@PS) and a heptafluoropropyl-substituent (C(3)F(7); nickel(II)-bis[(1R,4S)-3-heptafluorobutanoyl-10-propylenoxycamphor]-polysiloxane Ni(hfpc)(2)@PS) were synthesized, characterized and immobilized to polysiloxane. Ni(hfpc)(2)@PS was immobilized with a selector content of 38% and their enantioseparation ability was compared to selector concentrations of 4% and 20%. The influence of the perfluorinated moiety as well as the effect of the selector concentration on enantioseparations were investigated. Based on different functionalized organic compounds the quality of enantioseparation was analyzed and compared.

MATERIALS
Product Number
Brand
Product Description

Supelco
D-Camphor, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
(±)-Camphor, ≥95.5%
Sigma-Aldrich
(1R)-(+)-Camphor, 98%
Sigma-Aldrich
(±)-Camphor, SAJ first grade, ≥96.0%
Camphor (dl), primary reference standard
Camphor (racemic), European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
(±)-Camphor, purum, synthetic, ≥95.0% (GC)
Supelco
(−)-Camphor, analytical standard
Sigma-Aldrich
(±)-Camphor, meets analytical specification of Ph. Eur., BP, racemic, ≥95% (GC)
Sigma-Aldrich
Camphor, 96%
Sigma-Aldrich
D-Camphor, ≥97%, FG
Sigma-Aldrich
(1S)-(−)-Camphor, 95%