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  • 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

Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Sigma-Aldrich
1-Amino-2-methylpropan-2-ol, AldrichCPR
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Acetic acid-12C2, 99.9 atom % 12C
USP
Dehydrated Alcohol, United States Pharmacopeia (USP) Reference Standard
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Methanol, anhydrous, 99.8%
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
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Acetic acid, analytical standard
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Triethylamine, purum, ≥99% (GC)
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Methanol, analytical standard
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Ammonium acetate, LiChropur, eluent additive for LC-MS
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Diethanolamine, BioUltra, ≥99.5% (GC)
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Triethylamine, BioUltra, ≥99.5% (GC)
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Diethanolamine, puriss. p.a., ACS reagent, ≥99.0% (GC)
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Diethanolamine, analytical standard
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Triethylamine, for protein sequence analysis, ampule, ≥99.5% (GC)
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N,N-Diethylaniline, ≥99%
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Acetic acid, ≥99.5%, FCC, FG
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Ammonia, anhydrous, ≥99.98%
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Diethanolamine, ACS reagent, ≥98.5%
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Ammonium acetate, reagent grade, ≥98%
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Ammonium acetate, BioXtra, ≥98%
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Ammonia, puriss., anhydrous, ≥99.95%
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Ammonium acetate solution, for molecular biology, 7.5 M
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Ammonia solution, 0.4 M in THF
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Ammonium acetate, for molecular biology, ≥98%
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Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
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Ammonium acetate, 99.999% trace metals basis
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Triethylamine, for amino acid analysis, ≥99.5% (GC)
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Triethylamine, puriss. p.a., ≥99.5% (GC)
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Triethylamine, ≥99.5%