Skip to Content
Merck
  • Exploring the enantioseparation of amino-naphthol analogues by supercritical fluid chromatography.

Exploring the enantioseparation of amino-naphthol analogues by supercritical fluid chromatography.

Journal of chromatography. A (2015-02-18)
Anita Aranyi, István Ilisz, Antal Péter, Ferenc Fülöp, Caroline West
ABSTRACT

The direct separation of the enantiomers of 1-(α-aminoarylmethyl)-2-naphthol, 1-(α-aminoalkyl)-2-naphthol, 2-(α-aminoarylmethyl)-1-naphthol analogues and 2-(1-amino-2-methylpropyl)-1-naphthol) was investigated in supercritical fluid chromatography. Five commercially available chiral stationary phases based on immobilized polysaccharide chiral selectors (Chiralpak IA, IB, IC, ID and IE) were evaluated. Chiralpak IB was by far the most efficient to achieve the separation of these racemates and was further selected for optimization of elution conditions. The effects of column temperature (varying between 5 and 45 °C) and co-solvent added to carbon dioxide (methanol, ethanol, isopropanol and dichloromethane) were investigated. A particular attention was paid to mobile-phase additives. Several of them, acids, bases or salts (namely water, formic acid, acetic acid, trifluoroacetic acid, diethylamine, diethanolamine, triethylamine, triethanolamine, dimethylethanolamine, ammonia and ammonium acetate), were tested in order to improve peak shapes while maintaining selectivity. With the help of other achiral naphthol derivatives, the additive effects were examined.

MATERIALS
Product Number
Brand
Product Description

Millipore
Bifido Selective Supplement B, suitable for microbiology
Supelco
2-Propanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Sigma-Aldrich
Methanol solution, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Dichloromethane, Selectophore, ≥99.5%
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Sigma-Aldrich
2-Propanol, BioReagent, ≥99.5%
Sigma-Aldrich
Triethanolamine, reagent grade, 98%
Sigma-Aldrich
Triethanolamine, BioUltra, ≥99.5% (GC)
Supelco
Dichloromethane, analytical standard
Sigma-Aldrich
Triethanolamine, ≥99.0% (GC)
Sigma-Aldrich
2-Propanol, BioUltra, ≥99.5% (GC)
Supelco
2-Propanol, analytical standard
Supelco
Ethanol, standard for GC
Sigma-Aldrich
Triethanolamine, puriss., meets analytical specification of NF, ≥99% (GC)
Sigma-Aldrich
Ethanol, purum, secunda spirit, denaturated with 2% 2-butanone, S15, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Diethylamine, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Ethanol
Sigma-Aldrich
Ethanol, tested according to Ph. Eur.
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Sigma-Aldrich
Diethylamine, purified by redistillation, 99.5%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Diethylamine, ≥99.5%
Sigma-Aldrich
Triethanolamine, puriss. p.a., ≥99% (GC)
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Supelco
Trifluoroacetic acid, analytical standard
Sigma-Aldrich
2-Propanol, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Ethanol, BioUltra, ≥99.8%, (absolute alcohol, without additive, A15 o1)
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard