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ReproSil Chiral-NR is based on the ultrapure Reprosil 100 Silica. The chiral selector, an aromatic compound, is covalently bound and has a similar broad chiral generality comparable with polysaccharide-derived chiral stationary phases. Reprosil Chiral-NR is a brush-type phase with p-acceptor and p-donor groups, therefore the phase can be used for compounds which also contain p-acceptor and p-donor groups.
Due to the 100A° pores and the large 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. In preparative separations it is an advantage to get the minor enantiomer eluting first. Reprosil Chiral-NR-R shows the reversed elution order, because it is modified with the opposite enantiomeric chiral form compared to Reprosil Chiral-NR.
Both phases are stable in all commonly used eluents, including aqueous systems. Typical eluents in the normal-phase mode are mixtures of Hexane and 2-Propanol, in the reversed phase mode mixtures of MeOH and water. The ideal operating pH-range is between 2 und 7, and the columns are stable up to 300 bar. Very often one can use the same or similar eluents like on the polysaccharide-derived CSPs.
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 with both acids and with bases. ReproSil Chiral-NR allows the separation of underivatized racemates like: Amides, Alcohols, Aldehydes, Aziridines, Carbamates, Carboxylic acids, Epoxides, Esters, Ethers, Ketones, Phosphonates, Sulfonamides and Ureas.
Rule of thumb:
A good chiral separation can be expected with aromatic compounds with an Oxygen (or Nitrgen) at or very near to the chiral centre.
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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Abscisic acid: |
Eluent: Hexane / IPA (85/15) + 0,1 % Acetic acid |
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Anisoin: |
Eluent: Hexane / IPA (80/20) + 0,5 % Acetic acid |
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Benzoin: |
Eluent: Hexane / IPA (80/20) |
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Benzoyloxycarbonylalanin |
Eluent: Hexane / IPA (95/5) + 0,1 % TFA |
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Binaphthol: |
Eluent: Hexane / IPA (90/10) |
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Bupivacaine: |
Eluent: Hexane / IPA (80/20) + 0,1% TEA |
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Bromacil: |
Eluent: Hexane / IPA (98/2) |
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2-(pChlorphenyloxy) propionic |
Eluent: Hexane / IPA (95/5) + 0,1 % TFA |
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Cycloprofen: |
Eluent: Hexane / IPA (80/20) + 0,1 % Ammonium acetate |
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Cyclophosphamid: |
Eluent: Hexane / Ethanol (95/5) |
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Chlormezanone: |
Eluent: Hexane / IPA (60/40) |
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2,2’-Diamino-1,1’Binaphthyl |
Eluent: Heptane / Ethanol ( 90 / 10) |
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Dihydrotertabenazine: |
Eluent: Hexane / IPA (60/40) + 0,1 % TEA |
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Fenoprofen: |
Eluent: Hexane / IPA (98/2) + 0,1 % Acetic acid |
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FMOC-Alanine |
Eluent: Hexane / IPA (95/5) + 0,1 % TFA |
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Flavanon: |
Eluent: Hexane / IPA (99/1) |
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Hydrobenzoin: |
Eluent: Hexane / IPA (95/5) |
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Ibuprofenol: |
Eluent: Hexane / IPA (99/1) |
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Ibuprofen: |
Eluent: Hexane / IPA (90/10) + 0,01 % Ammonium acetate |
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Indapamide: |
Eluent: Hexane / IPA (50/50) |
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Ketamine: |
Eluent: Hexane / IPA (99/1) + 0,1 % TEA |
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Ketorolac: |
Eluent: Hexane / IPA (98/2) + 0,1 % TFA |
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Ketopropfen: |
Eluent: CH2Cl2 / Hexane / Ethanol (47/47/6) + 0,01 M Amm. acetate |
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Lorazepam: |
Eluent: Hexane / IPA (70/30) + 0,1 % Acetic acid |
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Loxoprofen: |
Eluent: Hexane / Ethanol (85/15) + 0,01 M Ammonium acetate |
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2-Methyl-1-Indanone: |
Eluent: Hexane / IPA (99/1 |
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Mecoprop: |
Eluent: Hexane / IPA (99/1) + 0,1 % Acetic acid |
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Metolazone: |
Eluent: Hexane / Ethanol (55/45) |
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a-Methoxyphenyl-Acetic acid: |
Eluent: Hexane / Ethanol (90/10) + 0,01 % Ammonium acetate |
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3-Methyl-5-Phenylhydantoin: |
Eluent: Hexane / IPA (90/10) |
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N-(1-(4-Bromo-Phenyl)-2-methylene-3-oxo-Butyl) –4-Methyl-Benzenesulfonamide: Heptane / Ethanol (90/10) Nadolol: |
Eluent: Hexane / Ethanol (78/22) + 0,01 M Ammonium acetate |
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2-(2-Naphthyloxy) proponic acid |
Eluent: Hexane / IPA (95/5) + 0,1 % TFA |
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Naproxen: |
Eluent: Hexane / IPA (60/40) + 0,1 % Acetic acid |
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Nicardipine: |
Eluent: Hexane / IPA (73/27) + 0,1 % Acetic acid |
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Nirvanol: |
Eluent: Hexane / IPA (80/20) |
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N,N-Phtaloylalanin |
Eluent: Hexane / IPA (95/5) + 0,1 % TFA |
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Ofloxacin: |
Eluent: CH2Cl2 / Hexane / Ethanol (43/43/14) + 0,01 M Amm. acetate |
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Oxazepam: |
Eluent: Hexane / IPA (75/25) + 0,01 % Ammonium acetate |
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Permethrin: |
Eluent : Hexane + 0,2 % IPA |
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2-Phenylcyclopropan-Carboxylat: |
Eluent: Hexane / IPA (99/1) |
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Proglumide: |
Eluent: Hexane / IPA (75/25) + 0,1 % Acetic acid |
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Propafenone: |
Eluent: CH2Cl2 / Hexane / 0,01 M Ammonium acetate (47/47/6) |
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Resmethrin: |
Eluent: Hexane |
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Styrene-Oxid: |
Eluent: Hexane / IPA (99/1) |
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Stilbene Oxid: |
Eluent: Heptane / IPA ( 85 / 15) |
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Sulfinpyrazone: |
Eluent: Hexane / Ethanol (75/25) + 0,15 M Ammonium acetate |
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Temazepam: |
Eluent: Hexane / IPA (80/20) + 0,1 % Acetic acid |
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Terfenadine: |
Eluent: Hexane / Ethanol (97/3) + 0,01 m Ammonium acetate |
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Tiaprofenic acid: |
Eluent: Hexane / IPA (80/20) + 0,1 % Acetic acid |
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Tolperisone: |
Eluent: Hexane / IPA (99/1) + 0,1 % TEA |
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Trolox: |
Eluent. Hexane / IPA (95/5) + 0,1 % Acetic acid |
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Vanilmandelic acid: |
Eluent: Hexane / Ethanol (85/15) + 0,01 M Ammonium acetate |
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Warfarin: |
Eluent: Hexane / IPA (65/35) + 0,1 % Acetic acid |
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Zopiclone: |
Eluent: CH2Cl2 / Ethanol (95/5) + 0,01 M Ammonium acetate |
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Reversed-Phase: |
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Isradipine: |
Eluent: MeOH / H20 (63/37) |
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Kynurenine: |
Eluent: MeOH / H20 (65/35) + 0,1 % Acetic acid |
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Mandelic acid: |
Eluent: H20 + 0,1 % Acetic acid |
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Naproxen: |
Eluent: MeOH / H20 (80/20) + 0,1 % Acetic acid |
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Nimodipine: |
Eluent: MeOH / H20 (65/35) |
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p-Chloro-Warfarin: |
Eluent: MeOH / H20 (85/15) + 0,1 % Acetic acid |
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Warfarin: |
Eluent: MeOH / H20 (70/30) + 0,1 % Acetic acid |
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Method development for Normal-Phase Separations:
1.) Start off with a mixture of Hexane / IPA (50/50).
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-NR, 8 µm, 250 x 4.6 mm, Part.No.: r18.nr.s2546 |
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