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Due to the 100A° pores and the big surface area of 350 m2/g the phase has an excellent preparative capacity. With a 250 x 10 mm column one can separate 50 – 250 mg / injection and with a 250 x 20 mm column 250 – 1000 mg/ injection.
The phase is stable in all commonly used normal phase eluents. Typical eluents are mixtures of Hexane and 2-Propanol. The best pH-range is between 2 und 7. The columns are stable up to 300 bar.
The peak shape of acids can be improved with 0,1 % acetic acid, the peak shape of bases with 0,1 % TEA. With 0,01% Ammonium Acetate a good peak shape can be achieved both with acids and with bases.
Examples for Separations:
The most commonly used column dimension is 250 x 4.6 mm with a flow of 1,5 ml / min
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Aromatic Alcohols: |
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Benzoin |
Eluent: Heptane / IPA ( 99/1) |
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tert-Butyl-Phenyl-Carbinol: |
Eluent: Heptane / IPA (99/1) |
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-Naphthyl-Methyl-Carbinol: |
Eluent: Hexane / IPA (99/1) |
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9-Anthryl-Trifluoromethyl-Carbinol: |
Eluent: Hexane / IPA (95/5) |
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Acenaphthenol: |
Eluent: Hexane / IPA (95/5) |
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1,1’-2-Binaphthol: |
Eluent: Hexane / IPA + 0.1 % TFA (98/2) |
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9-Anthrylethanol: |
Eluent: Heptane / IPA (95/5) |
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1-Naphthyl-2-Butanol: |
Eluent: Heptane / IPA (95/5) |
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2-Naphthyl-2-Butanol: |
Eluent: Heptane / IPA (95/5) |
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1-Phenylpentanol: |
Eluent: Heptane / 1,2-Dimethoxyethane (99/1) |
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Phenyl-Tribromomethyl-Carbinol: |
Eluent: Hexane / IPA (99/1) |
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Phenyl-Methyl-Carbinol: |
Eluent: Hexane 100 % |
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Phenyl-Ethyl-Carbinol: |
Eluent: Hexane / IPA (99/1) |
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1,1,2-Triphenyl-1,2-Ethandiol: |
Eluent: Heptane / IPA (99/1) |
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1,1’-Binapthol-Monomethylether: |
Eluent: Hexane / IPA + 0,1 % TFA (98/2) |
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trans-Phenyl-Cyclohexanol: |
Eluent: Heptane / IPA (99/1) |
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Phenyl-Cyclohexyl-Carbinol: |
Eluent: Heptane / IPA (99/1) |
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Phenyl-Isopropyl-Carbinol: |
Eluent: Heptane / IPA (99/1) |
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Phenyl-Phenylethyl-Carbinol : |
Eluent: Heptane / IPA (99/1) |
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1-Phenyl-2-Propanol: |
Eluent: Heptane / 1,2-Dimethoxyethane (98.5/1.5) |
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3-Thiophenethanol: |
Eluent: Heptane / 1,2-Dimethoxyethane (98.5/1.5) |
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1-(o-Methoxyphenyl)-Ethanol: |
Eluent: Heptane / 1,2-Dimethoxyethane (98.5/1.5) |
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1-(4-Phenyl)-Phenylethanol: |
Eluent: Heptane / 1,2-Dimethoxyethane (98.5/1.5) |
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1-(p-Methylphenyl)-Ethanol: |
Eluent: Heptane / 1,2 Dimethoxyethane (98.5/1.5) |
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1-(p-Chlorophenyl)-Ethanol: |
Eluent: Heptane / 1,2 Dimethoxyethane (98.5/1.5) |
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Vapol: |
Eluent: 100 % Methanol |
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Warfarin: |
Eluent: Heptane / IPA + 0,1 % TFA (70/30) |
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Other Racemate-groups: |
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Flobufen: |
Eluent: Heptane / IPA + 0.1 % TFA (90/10) |
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Trichlormethiazide: |
Eluent: Hexane / IPA + 0.1 % Acetic acid (75/25) |
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Prilocaine |
Eluent: Hexane / Ethanol + 0,01M Ammonium acetate (99/1) |
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Etodolac: |
Eluent: Hexane / IPA + 0,1 % TFA (98/2) |
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Naproxen : |
Eluent: Heptane / IPA + 0,1 % TFA (90/10) |
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Phenylbutyric acid: |
Eluent: Heptane / IPA + 0,1 % TFA (99/1) |
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Trolox: |
Eluent: Hexane / IPA + 0,1 % Acetic acid (95/5) |
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Ditoluoyltartaric acid: |
Eluent: Hexane / IPA + 0,1 % TFA (90/10) |
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Phenylsuccinic acid: |
Eluent: Hexane / IPA + 0.1 % TFA (95/5) |
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1-Cyclopentyl-1-Phenylacetic acid: |
Eluent: Hexane / IPA + 0,1 % TFA (99/1) |
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Cyclopentyl-Benzoyl-Diamide: |
Eluent: Hexane / IPA (90/10) |
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Indapamide: |
Eluent: Hexane / IPA (75/25) |
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Thalidomide: |
Eluent: Hexane / IPA + 0,1 % Acetic acid (90/10) |
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Bendroflumethiazide: |
Eluent: Hexane / IPA (75/25) |
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Cyclothiazide: |
Eluent: Hexane / IPA + 0,1 % Acetic acid (75/25) |
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Method development for Normal-Phase Separations: |
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1.) Start off with a mixture of Hexane / IPA (90/10).
2.) If the RT is too short, add less IPA; if the RT is too long, add more IPA.
3.) Peak-Tailing
with acids: use 0,1 % Acetic acid,
with bases: use 0,1 % TEA.
You can improve the peak shapes in both cases with 0,01 % Ammonium acetate.
4.) The method can be further optimized by replacing Hexane with Heptane and / or IPA with Ethanol.
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Examples : Reprosil Chiral-OH, 8 µm, 250 x 4.6 mm, Art.Nr.: r18.OH.s2546 |
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