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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

USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Ethanol, BioUltra, for molecular biology, ≥99.8%, (absolute alcohol, without additive, A15 o1)
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1-Amino-2-methyl-2-propanol, 95% anhydrous basis
Supelco
Triethanolamine, analytical standard
USP
2-Propanol, United States Pharmacopeia (USP) Reference Standard
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Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
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2-Propanol, Laboratory Reagent, ≥99.5%
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Isopropyl alcohol, meets USP testing specifications
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2-Propanol, ACS reagent, ≥99.5%
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Ethanol, purum, absolute ethanol, denaturated with 4.8% isopropanol, A15 IPA1, ≥99.8% (based on denaturant-free substance)
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Ethanol, ACS reagent, prima fine spirit, without additive, F15 o1
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Ethanol, purum, absolute ethanol, denaturated with 2% 2-butanone, A15 MEK1, ≥99.8% (based on denaturant-free substance)
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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
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Ethanol, purum, fine spirit, denaturated with 4.8% methanol, F25 METHYL1, ~96% (based on denaturant-free substance)
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Ethanol, purum, absolute ethanol, denaturated with 1% cyclohexane, A15 CYCLO1, ≥99.8% (based on denaturant-free substance)
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Trifluoroacetic acid, ReagentPlus®, 99%
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2-Propanol, ACS reagent, ≥99.5%
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Formic acid, ACS reagent, ≥96%
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Dichloromethane, biotech. grade, 99.9%, contains 40-150 ppm amylene as stabilizer
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Formic acid, ACS reagent, ≥88%
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2-Propanol, puriss. p.a., ACS reagent, ≥99.8% (GC)
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Dichloromethane, puriss., meets analytical specification of Ph. Eur., NF, ≥99% (GC)
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Ethyl alcohol, Pure, 200 proof, HPLC/spectrophotometric grade
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Ethanol, absolute, reag. ISO, reag. Ph. Eur., ≥99.8% (GC), liquid (clear, colorless)
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Ethyl alcohol, Pure, 200 proof, ACS reagent, ≥99.5%
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Ethyl alcohol, Pure, 200 proof, meets USP testing specifications
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2-Propanol, puriss., meets analytical specification of Ph. Eur., BP, USP, ≥99.5% (GC)
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2-Propanol, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
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Trifluoroacetic acid, suitable for HPLC, ≥99.0%