Finding the best separation for enantiomeric mixtures
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Finding the best separation for enantiomeric mixtures
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Finding the best separation for enantiomeric mixtures
- 1. Finding the best separation for enantiomeric mixtures Chiral Technologies Europe Illkirch Cedex – France Chiral Technologies, Inc. West Chester, PA
- 3. Method Development Overview for Polysaccharide-derived CSPs Racemic mixture HPLC SFC Organic mobile phases Water compatible mobile phases CHOICE OF SEPARATION MODE CHOICE OF TECHNOLOGY
- 6. HPLC method development in organic mobile phases
- 11. Basic Molecule – Analytical Scale IA IB IC Hept/EtOH/DEA Hept/IPA/DEA Hept/THF/DEA Hept/DCM/DEA Separation Retention time > 30 min Separation Retention time > 30 min 70/30/0.1 70/30/0.1 90/10/0.1 80/20/0.1 Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -50 0 50 100 150 200 250 300 350 400 450 mAU -50 0 50 100 150 200 250 300 350 400 450 1: 290 nm, 4 nm CE070128 - IA - Heptane-EtOH - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU 0 50 100 150 200 250 300 mAU 0 50 100 150 200 250 300 1: 290 nm, 4 nm CE070128 - IA - Heptane-IPA - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -2,5 0,0 2,5 5,0 7,5 10,0 12,5 15,0 17,5 20,0 22,5 25,0 mAU -2,5 0,0 2,5 5,0 7,5 10,0 12,5 15,0 17,5 20,0 22,5 25,0 1: 290 nm, 4 nm CE07128 - IA - Hept-THF 90-10-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -5 0 5 10 15 20 25 30 mAU -5 0 5 10 15 20 25 30 1: 290 nm, 4 nm CE07128 - IA - Hept-DCM 80-20-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -50 0 50 100 150 200 250 300 350 400 450 mAU -50 0 50 100 150 200 250 300 350 400 450 1: 290 nm, 4 nm CE070128 - IB - Heptane-EtOH - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -25 0 25 50 75 100 125 150 175 200 225 250 275 mAU -25 0 25 50 75 100 125 150 175 200 225 250 275 1: 290 nm, 4 nm CE070128 - IB - Heptane-IPA - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -50 0 50 100 150 200 250 300 350 400 450 mAU -50 0 50 100 150 200 250 300 350 400 450 1: 290 nm, 4 nm CE070128 - IC - Heptane-EtOH - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -25 0 25 50 75 100 125 150 175 200 225 250 mAU -25 0 25 50 75 100 125 150 175 200 225 250 1: 290 nm, 4 nm CE070128 - IC - Heptane-IPA - 70-30-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -2,5 0,0 2,5 5,0 7,5 10,0 12,5 15,0 17,5 20,0 22,5 25,0 mAU -2,5 0,0 2,5 5,0 7,5 10,0 12,5 15,0 17,5 20,0 22,5 25,0 1: 290 nm, 4 nm CE07128 - IC - Hept-THF 90-10-Rep2 Retention Time Minutes 0 2 4 6 8 10 12 14 16 18 20 22 24 mAU -10 0 10 20 30 40 50 mAU -10 0 10 20 30 40 50 1: 290 nm, 4 nm CE07128 - IC - Hept-DCM 80-20-Rep2 Retention Time
- 12. Basic Molecule – Analytical Scale CHIRALPAK IB n -heptane/2-PrOH/DEA 70/30/0.1 12 min 7 min
- 15. SFC method development in organic mobile phases
- 18. CSPs in SFC: Analytical Scale CO 2 / MeOH 90/10 T=25°C Flow rate: 3.0ml/min. CHIRALPAK IA CO 2 / THF (+1%DEA) 70/30 T=30°C Flow rate: 3.0ml/min. CHIRALPAK IC 0 200 400 600 800 1000 1200 (sec)
- 20. HPLC method development in water compatible mobile phases
- 21. Water Compatible Mobile Phases Aqueous Solution Organic modifier Identify the compound nature Acidic Neutral Basic HCOOH pH 2.0 40% ACN 60% MeOH H 2 O 40% ACN 60% MeOH 20mM NH 4 HCO 3 pH 9.0 40% ACN 60% MeOH
- 22. Separations RP-Mode CHIRALPAK IA furoin MeOH/H 2 O 55:45 min 0 2 4 6 8
- 23. Separations RP-Mode CHIRALPAK IC 2,3-dibenzoyl- DL-tartaric acid HCOOH aq. (pH2.0) ACN: 55% min 0 2 4 6 8
- 24. Faster screening and enhanced resolution: 3-µm CSPs
- 25. Fast Analysis: CHIRALPAK IA-3 (4.6 x 50 mm) Hexane-EtOH 80:20 (+0.1% AE) Flow rate: 5.0 ml/min DCM-MeOH 98:2 (+0.1% AE) Flow rate: 5.0 ml/min MeOH 100% Flow rate: 5.0 ml/min 40 seconds 30 seconds 20 seconds
- 26. Looking for new separations: different chiral selectors
- 27. Different Substituents; New Enantiorecognition CHIRALCEL OD CHIRALPAK AD CHIRALCEL OZ CHIRALPAK AZ CHIRALPAK IC CHIRALPAK AY
- 28. Are New Selectors Needed? Metolachlor Hexane / EtOH 95:5 1ml/min, 25°C (4.6 x 250 mm) CHIRALPAK IA CHIRALPAK IB CHIRALPAK IC CHIRALPAK IA CHIRALPAK IB CHIRALPAK IC
- 29. Are New Selectors Needed? Metolachlor Hexane / EtOH 95:5 1ml/min, 25°C (4.6 x 250 mm) CHIRALPAK AS-H CHIRALPAK AD-H CHIRALCEL OD-H CHIRALCEL OJ-H
- 30. Are New Selectors Needed? Metolachlor Hexane / EtOH 95:5 1ml/min, 25°C (4.6 x 250 mm) CHIRALPAK AY-H
Notas do Editor
- Speak the line, “Can we achieve this with a minimal number of columns and efficient screening strategies?”
- Speak, “Analytical, but also preparative considerations.”
- Speak, « Looking for a given elution order »
- Speak that these are Polysacchasride-derived CSPs Also speak: « These will irreversibly destroy coated CSPs »
- Speak « These will irreversibly destroy coated CSPs »
- Speak, “An alternative possibility would be using polar organic mode to be water compatible.”
- Different substituents New enantiorecognition