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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

Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
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Formic acid, ≥95%, FCC, FG
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Ethanol, absolute, sales not in Germany, ≥99.8% (vol.)
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Triethanolamine, reagent grade, 98%
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2-Propanol, BioUltra, Molecular Biology, ≥99.5% (GC)
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Dichloromethane, Selectophore, ≥99.5%
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Ethanol, purum, secunda spirit, denaturated with 2% 2-butanone, S15, ~96% (based on denaturant-free substance)
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Ethanol, standard for GC
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2-Propanol, analytical standard
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Triethanolamine, puriss., meets analytical specification of NF, ≥99% (GC)
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Diethylamine, puriss. p.a., ≥99.5% (GC)
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Ethanol
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Trifluoroacetic acid, analytical standard
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5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
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Formic acid solution, BioUltra, 1.0 M in H2O
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Diethylamine, purified by redistillation, 99.5%
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Triethanolamine, BioUltra, ≥99.5% (GC)
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Triethanolamine, puriss. p.a., ≥99% (GC)
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Triethanolamine, ≥99.0% (GC)
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2-Propanol, BioReagent, ≥99.5%, Molecular Biology
Millipore
Bifido Selective Supplement B, suitable for microbiology
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2-Propanol, Pharmaceutical Secondary Standard; Certified Reference Material
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Diethylamine, ≥99.5%
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Ethanol, tested according to Ph. Eur.
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Ethanol, purum, absolute ethanol, denaturated with 4.8% isopropanol, A15 IPA1, ≥99.8% (based on denaturant-free substance)
Supelco
Dichloromethane, analytical standard
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5α-Androstan-17β-ol-3-one, ≥97.5%
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2-Propanol, puriss. p.a., ACS reagent, ≥99.8% (GC)
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Ethanol, purum, fine spirit, denaturated with 2% 2-butanone, F25 MEK1, ~96% (based on denaturant-free substance)
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Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer