TCI Chiral HPLC Column

TCI Chiral HPLC Column ~ Helical Polymer New Chiral Stationary Phase ~ Tokyo Chemical Industry Co.,Ltd. 212 Tokyo Chemical Industry Co., Ltd.

Features of TCI Chiral A unique new stationary phase Polymaleimide helical polymer bearing chiral side groups coated on silica gel. Suitable for separation of carbonyls and others Ex. Ketones, Esters, Carboxylic acids, N-Protected Amino acid, Alcohols and others. Applicable to both normal and reversed phase modes. High column load capacity Superior column longevity Maximum pressure: 29 psi (2 MPa) High throughput analysis Affordable price 212 Tokyo Chemical Industry Co., Ltd.

Line Up Column TCI Chiral MB-S TCI Chiral BP-S TCI Chiral CH-S Ligand N N N N N N Retention Power (Normal Phase) High Medium Weak Analyte Low polar Medium polar High polar Carbonyls (Ketones. Esters, Carboxylic acids, N-Protected amino acids),alcohols, Diols, Epoxides, Heterocycles, Sulfoxides, thers 212 Tokyo Chemical Industry Co., Ltd.

Applications Column TCI Chiral MB-S TCI Chiral BP-S TCI Chiral CH-S Separation % of 81compounds 9% 76% 71% N-Boc-prolinol 1 4 9 8 7 6 4 3 3 2 2 1 1. 2.. 7. min 1. 2.. 7. min 9 8 7 6 4 3 2 Applications 11 1 9 8 7 6 3 3 2 1 1 No Separation No Separation 1,1 -Bi-naphthol DL-Lactide 1.. 1. 1. 2.. min No Separation.. 1. 1. min No Separation 2 mv 17 1 1 1 7.. 1. 1. min Please see next and after the next pages as examples. All chromatograms are on our web site. 212 Tokyo Chemical Industry Co., Ltd.

Separation Compounds 1 212 Tokyo Chemical Industry Co., Ltd.

Separation Compounds 2 212 Tokyo Chemical Industry Co., Ltd.

Analytical condition Normal Phase n-hexane / IPA = 9/1 (initial condition) Elution time is long increase IPA ratio (ex.3%) Elution time is short decrease IPA ratio (ex.1%) Acidic compound add.1% of Trifluoroacetic acid Basic compound add.1% of Diethylamine Reversed Phase Acetonitrile / Water = 2/8 (initial condition) Elution time is long increase acetonitrile ratio (ex.4%) Elution time is short decrease acetonitrile ratio (ex.1%) Acidic compound add.1% of Trifluoroacetic acid Basic compound choice buffer solution Unusable solvents THF, Toluene, Halogenated solvents (Chloroform, etc.) 212 Tokyo Chemical Industry Co., Ltd.

Change ratio of solvents Change retention power Hexane/IPA=2/1(v/v) Hexane/IPA=1/1(v/v) Hexane/IPA=9/(v/v) Hexane/IPA=9/1(v/v) Column : TCI Chiral MB-S (3μm) Column Size : 4.6 mmi.d. mm Mobile Phase : Hexane/IPA Detection : UV 4 nm Flow Rate : 1. ml/min Temperature : 4 Sample : Benzoin Hexane/IPA=8/1(v/v) Hexane/IPA=8/2(v/v) Hexane/IPA=7/3(v/v) 212 Tokyo Chemical Industry Co., Ltd.

Temperature effect 19 Column : TCI Chiral MB-S (3μm) Column Size : 4.6 mmi.d. mm Mobile Phase : Hexane/IPA = 9/1 (v/v) Detection : UV 4 nm Flow Rate : 1. ml/min Temperature : 4 Sample : Benzoin 4 212 Tokyo Chemical Industry Co., Ltd.

Modifier effect Column : TCI Chiral MB-S (3μm) Column Size : 4.6 mmi.d. mm Mobile Phase : Hexane / Polar Solvent = 9/1 Detection : UV 4 nm Flow Rate : 1. ml/min Temperature : 4 Sample : Benzoin Benzoin EtH Pressure:.6MPa IPA Pressure:.7MPa MTBE Pressure:.3MPa MTBE : Methyl tert-butyl ether 212 Tokyo Chemical Industry Co., Ltd.

Stability test uv 2 Column : TCI Chiral BP-S Column Size : 4.6mmID mm Mobile Phase 2 : Hexane/IPA = 9/1 Detection : UV 4 nm Flow Rate 17:.7 ml/min Temperature : 4 Sample : Benzoin 1 injection α Rs 1 2.13 2.41 4 2.14 2.3 6 2.13 2.32 8 2.12 2.3 1 2.12 2.29 Injection:1 1 Injection:4 1 Injection:6 7 Injection:8 Injection:1.. 1. 1. 2. 2. 3. 3. 4. 4. min 212 Tokyo Chemical Industry Co., Ltd.

Batch to batch reproducibility alpha 2. 2 1. 1 Benzoin 1-Phenyl-1,2- ethandiol. 1st 2nd 3rd 4th th 6th 7th TCI Chiral MB-S (3μm) 212 Tokyo Chemical Industry Co., Ltd.

Column load capacity test Analysis 12. 1. 7.. 2.. 2 1 2 3 4 min Column Size : 4.6mmI.D. mm Flow Rate : 1. ml/min Sample Load:.mg 1 2 3 4 Time(min) Loading test by analysis column Column Size : 4.6mmI.D. mm Flow Rate : 1. ml/min N-Cbz-proline Column Mobile Phase Temperature : 4ºC Detection : UV4nm Loading test by prep column N H : TCI Chiral MB-S (µm) : n-hexane/2-propanol/tfa =9/1/.1 Column Size : 2.mmI.D. mm Flow Rate : 9. ml/min 1 1 Sample Load: 2mg Sample Load: 4mg 1 2 3 4 min 1 2 3 4 Time(min). 2. 4. 6. 8. 1. 12. 14. 3 6 9 12 Time(min) 212 Tokyo Chemical Industry Co., Ltd.

N-Protected alanine applications N-Acetyl N-BC N-CBZ N-FMC Alpha 1.9 1.7 2.6 3.3 Rs 8.9 2.4 11. 13. 8 7 6 4 3 N-Acetyl alanine 1 1 7 Column : TCI Chiral BP-S (μm) Column Size : 4.6mmID mm Mobile Phase : Hexane/IPA/TFA=9//.1 Detection : UV21nm (N-Acetyl, N-BC) UV4nm (N-CBZ, N-FMC) Flow Rate : 1.mL/min Temperature : 4 N-BC alanine 2 1.. 1. 1. 2.. min 2. 2.. 7. min 1 1 N-CBZ alanine 2 1 1 N-FMC alanine 1 2 3 4 min.. 1. 1. 2.. min 212 Tokyo Chemical Industry Co., Ltd.

Comparison with Polysaccharide types Carvone 1,4-Di--benzylthreitol 3 2 1 1 4 4 3 3 2 1 4 4 3 3 2 1 H H CH 2 CH 2 Ph 12. H H 1. 7. CH 2 CH 2 Ph. 1 1 2.. 2.. 7. min 4 4 3 TCI Chiral MB-S. 2.. 7. min 7 6 Amylose type 1. 2.. 7. min TCI Chiral MB-S 9 8 7. 3 3 1 2 3 4 min Amylose type 1 3 6 4 2 2 1 1. 2.. 7. min TCI Chiral BP-S 3 2 1 Amylose type 2. 2.. 7. min 4 3 2 1 9. 2.. 7. min TCI Chiral BP-S 1 1 9 1 2 3 4 min Amylose type 2 4 7 8 8 3 6 7 7 3 2 1 4 3 6 4 3 6 4 3 1 2 2 2 1 1 1 TCI Chiral CH-S. 2.. 7. min Cellulose type. 2.. 7. min. 2.. 7. min TCI Chiral CH-S 1 2 3 4 min Cellulose type 212 Tokyo Chemical Industry Co., Ltd.

4 4 3 3 2 1 1 9 8 7 6 4 3 2 1 8 7 6 4 3 2 1.. 1. 1. min.. 1. 1. min 9.. 1. 1. min Comparison with Polysaccharide types Guaiacol Glycerol Ether 2 1 1 4 3 2 1 22. 2. 17. 1. 12. 1. 7.. 2.. H H.. 1. 1. min 6.. 1. 1. min 1 2 3 4 min 7.. 2.. 1. 12. 1. 7.. 2.. 1. 7.. 2.. -2. -. 1 2 3 4 min.. 1. 1. 2.. min Mevalonolactone.. 1. 1. min 3. 3. 2. 2. 1... 4 3 2 1-1 -2-3 22. 2. 17. 1. 12. 1. 7.. 2.. -2... 1. 1. 2.. min TCI Chiral MB-S Amylose type 1 TCI Chiral MB-S Amylose type 1 H 1... 1. 1. 2.. min TCI Chiral BP-S Amylose type 2 TCI Chiral BP-S Amylose type 2.. 1. 1. 2.. min TCI Chiral CH-S Cellulose type TCI Chiral CH-S Cellulose type 212 Tokyo Chemical Industry Co., Ltd.

Comparison with Polysaccharide types 2 1 1 Butyl Lactate H 1. 12. 1. 7.. 2. 17. 1. 12. 1. 7.. 2. Glycidyl p-toluenesulfonate S 3 3 2 1 1. 2.. 7. min 3. 2.. 7. min 3 2 1 1. 2.. 7. min... 2.. 7. min.. 1. 1. 2.. min.. 1. 1. 2.. min TCI Chiral MB-S Amylose type 1 TCI Chiral MB-S Amylose type 1 3 4 8 3 7 4 3 6 2 3 1 2 2 4 1 3 1 1 1 2 1. 2.. 7. min 6 4 3 2 1. 2.. 7. min 4.. 1. 1. 2.. min.. 1. 1. 2.. min 9 8 7 7 6 6 4 4 3 3 2 2 1 1.. 1. 1. 2.. min TCI Chiral BP-S Amylose type 2 TCI Chiral BP-S Amylose type 2.. 1. 1. 2.. min TCI Chiral CH-S Cellulose type TCI Chiral CH-S Cellulose type 212 Tokyo Chemical Industry Co., Ltd.

Comparison with Polysaccharide types 1 1 1 7 1 2-Chloropropionic Acid Cl. 2.. 7. min TCI Chiral MB-S 7 H. 2.. 7. min 9 Amylose type 1 2 2 17 1 1 1 7 4-Isopropyl-3-propionyl-2- oxazolidinone 9 1 2 3 4 min TCI Chiral MB-S 8 7 6 N 4 3 2 1. 2.. 7. min Amylose type 1 1 1 7 8 7 6 4 3 1 7 1 7 2 1. 2.. 7. min TCI Chiral BP-S -1. 2.. 7. min 1 Amylose type 2. 2.. 7. min TCI Chiral BP-S. 2.. 7. min Amylose type 2 1 1 1 1 1 7 7 7 7 -. 2.. 7. min TCI Chiral CH-S -.. 1. 1. min Cellulose type. 2.. 7. min TCI Chiral CH-S. 2.. 7. min Cellulose type 212 Tokyo Chemical Industry Co., Ltd.

SFC application CH C CH 2 H Benzyl DL-Mandelate 1. 2.. 3. Time(min.) Column : TCI Chiral MB-S (3µm) Column Size : 4.6mmID 1mm Temperature : 4ºC Pressure : 2MPa Mobile Phase : C 2 /IPA=9/1 Detection : UV4nm Flow Rate : 2.mL/min Sample : Benzyl DL-Mandelate.99mg/mL(IPA) Injection Vol. : µl Column Pressure: 2.4MPa SFC : Supercritical Fluid Chromatography 212 Tokyo Chemical Industry Co., Ltd.

Complete TCI Chiral product line Column Type TCI Chiral MB-S TCI Chiral BP-S TCI Chiral CH-S Particle Size 3μm μm 3μm μm 3μm μm 4.6mm mm S381 S384 S38 S38 S383 S386 4.6mm 1mm S381 S384 S382 S38 S383 S386 4.6mm mm S3811 S3841 S3821 S381 S3831 S3861 Cartridge type guard for 4.6mm column (3.mm 1mm) S3849(1/Pack) S389(1/Pack) S3869(1/Pack) 2.mm mm S3816 S3846 S3826 S386 S3836 S3866 2.mm 1mm S3812 S3842 S3822 S382 S3832 S3862 2.mm mm S3813 S3843 S3823 S383 S3833 S3663 Guard for 2. (or 4.6mm ) Column (1.mm 1mm ) S3819(3/Pack) S3829(3/Pack) S3839(3/Pack) 1.mm mm - S387 - S388 - S389 2.mm mm - S3871 - S3881 - S3891 3.mm 1mm guard column is a cartridge type column and needs a holder. Holder:S14 212 Tokyo Chemical Industry Co., Ltd.