HPLC Column for Structual Isomers

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Dominick Ward
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1 PLC Column for Structual Isomers lica Gel Average Particle ze Average Pore ze Stationary Phase Main Interaction Carbon Content CSMSIL PYE CSMSIL PE igh Purity Porous Spherical lica 2-(1-Pyrenyl)ethyl Group ydrophobic Interaction - Interaction Charge Transfer Interaction Stereoselectivity approx. 18% 5 μm approx. 120 A itrophenylethyl Group ydrophobic Interaction - Interaction Dipole-Dipole Interaction approx. 9% 3 C 3 C PYE 2 PE CSMSIL PYE (Pyrenylethyl group bonded) and CSMSIL PE (itrophenylethyl group bonded) column show unique retention characteristics based on multiple separation modes such as hydrophobic, charge transfer and - interactions. These columns are recommended for the separation of structural isomers. Pyrenylethyl group bonded stationary phase Separation with high molecular shape selectivity or - interactions Excellent separation for structural isomers CSMSIL PYE column is a reversed phase column with 2-(1-Pyrenyl) ethyl groups bonded silica packing material. This column utilizes - interactions originating from the planar pyrene ring structure to separate structural isomers. Separation of PAs Due to the planar pyrene ring structure and strong - interactions, CSMSIL PYE achieves excellent separation of aromatic isomers. 1. Benz [a] anthracene 2. Chrysene CSMSIL Conventional DS A: Water, B: Methanol B 80% B 100% 20 min. Linear Gradient 1. aphthalene 2. Acenaphthylene 3. Acenaphthene 4. Flourene 5. Phenathrene 6. Acnthracene 7. Fluoranthene 8. Pyrene 9. 2, 3-Benzofluorene 10. Benz [a] Anthracene 11. Chrysene 12. Triphenylene 13. aphthacene 14. Benzo[a] Pyrene 15. Perylene 16. Dibenz [a,c] Anthracene 17. Dibenz [a,h] Anthracene Methanol : Water = 90 : Benz [a] Anthracene 2. Chrysene

2 CSMSIL PYE (continued) Application Data Separation of Sterols AP Methanol : 2 = 98 : 2 AP Methanol : 2 = 90 : 10 Methanol : 2 = 95 : 5 UV 210 nm 1. Cholesterol 2. Stigmasterol 3. Campesterol 4. tosterol (5.6 μg) (5.9 μg) R R= 1; 3C 3; 3C C3 2; 3C 3C C3 4; Separation of Phthalonitriles AP o,p Methanol : 2 = 30: 70 AP Methanol : 2 = 50 : 50 Methanol : 2 = 80 : 20 ; ; ; Phthalonitrile Isophthalonitrile Terephthalonitrile (0.3 μg) (3.0 μg) (0.15 μg) Separation of Tocopherols AP Methanol : 2 = 95 : 5 AP Methanol : 2 = 90 : 10 Methanol : 2 = 90 : 10 UV 295 nm (R1:Me, R2:Me) (R1:Me, R2:) (R1:, R2:Me) (R1:, R2:) R 2 3C R 1 3 C 3 C Separation of Capsaicin AP Column size Mobile phase Flow rate Methanol : Water = 70 : 30 UV 280 nm 1. Capsaicin 2. -Vanillylnonanamide (1.0 g) (0.5 g) C3 C 3 Capsaicin C3 -Vanillylnonanamide

itrophenylethyl group bonded stationary phase Separation with dipole-dipole and - interactions Excellent separation for structural isomers Advantage of Dipole-Dipole Interactions The chromatogram

3 CSMSIL PE column is a reversed phase column with itrophenylethyl groups bonded silica packing material. This column provides unique retention characteristics, slightly different from the CSMSIL PYE column, utilizing both dipole-dipole and - interactions. itrophenylethyl group bonded stationary phase Separation with dipole-dipole and - interactions Excellent separation for structural isomers Advantage of Dipole-Dipole Interactions The chromatogram below illustrates the separation of,, tolunitrile. nce hydrophobic interaction is dominant in the separation by a DS column, tolunitrile elutes first. In CSMSIL PE, tolunitrile elutes later. This suggests that CSMSIL PE utilizes the interaction between -electron of the nitrophenyl group and - for retention in addition to hydrophobic interaction., Methanol : Water = 50 : 50 T B B T Tolunitrile (,, ) Benzene (B) Toluene (T) Application of Disubstituted aphtalenes CSMSIL PE strongly retains 1,8-dinitronaphthalene because of the strong dipole formed by the two nitro groups positioned on the same side of naphthalene. PYE: Methanol : Water = 90 : 10 PE: Methanol : Water = 70 : 30 DS: Methanol : Water = 80 : ,8-Dinitronaphtalene 2. 1,5-Dinitronaphtalene 3. aphtalene 4. 1-Methylnaphtalene 5. 1,5-Dimethylnaphtalene Effect of Dipole-Dipole Interaction The DS column cannot sharply separate the positional isomers like phthalonitriles. In contrast, CSMSIL PYE and PE can separate them very well by - interaction. Furthermore, CSMSIL PE strongly retains ortho compound which has a big dipole moment. o, PE: Methanol : Water = 40 : 60 PYE: Methanol : Water = 80 : 20 DS: Methanol : Water = 30 : Phthalonitrile (0.30 μg) 2. Phthalonitrile (3.00 μg) 3. Phthalonitrile (0.15 μg)

CSMSIL PE (continued) Application Data Positional Isomers like Benzylpyridines Methanol : 20 mmol/l K2P4 = 60 : 40 1. 2-Benzylpyridine 2. 3-Benzylpyridine 3.

0 mm I.D. x 250 mm 4.6 mm I.D. x 250 mm 10.0 mm I.D. x 250 mm 20.0 mm I.D. x 250 mm CSMSIL 1.0 mm I.D. x 150 mm Packed Column 2.0 mm I.D. x 150 mm 2.0 mm I.D. x 250 mm 4.6 mm I.D. x 250 mm 10.0 mm I.D. x 250 mm 20.0 mm I.D. x 250 mm ther size may be available.

4 CSMSIL PE (continued) Application Data Positional Isomers like Benzylpyridines Methanol : 20 mmol/l K2P4 = 60 : Benzylpyridine 2. 3-Benzylpyridine 3. 4-Benzylpyridine Geometrical Isomers like Carvylacetates 70% Methanol UV 215 nm 1. Carvylacetate (cis, trans) C rdering Information Product ame CSMSIL 1.0 mm I.D. x 150 mm Packed Column 2.0 mm I.D. x 150 mm 2.0 mm I.D. x 250 mm 4.6 mm I.D. x 250 mm 10.0 mm I.D. x 250 mm 20.0 mm I.D. x 250 mm CSMSIL 1.0 mm I.D. x 150 mm Packed Column 2.0 mm I.D. x 150 mm 2.0 mm I.D. x 250 mm 4.6 mm I.D. x 250 mm 10.0 mm I.D. x 250 mm 20.0 mm I.D. x 250 mm ther size may be available. Please enquire. Product umber Product ame CSMSIL Guard Column CSMSIL Guard Column 4.6 mm I.D. x 10 mm 10.0 mm I.D. x 20 mm 20.0 mm I.D. x 20 mm 20.0 mm I.D. x 50 mm 4.6 mm I.D. x 10 mm 10.0 mm I.D. x 20 mm 20.0 mm I.D. x 20 mm 20.0 mm I.D. x 50 mm Product umber For research use only, not intended for diagnostic or drug use. ACALAI TESQUE, IC. ijo Karasuma, akagyku Kyoto , JAPA TEL FAX Website (0) : +81-(0) : : info.intl@nacalai.com 1004

5 I. PLC Columns CSMSIL PYE Pyrenylethyl group bonded stationary phase Excellent separation for structural isomers II. UPLC Columns C18-MS- Cholester PE-MS - πap III. Preparative Packing Materials PYE α itrobenzene/benzene), 50%Methanol C 3 C 3 C PE-MS PYE IV. Related Products V. Applications Applications CSMSIL Application Data Mobile phase: Methanol/ 2 = 98/2 AP Methanol/ 2 = 90/10 Methanol/ 2 = 95/5 Flow rate: : 30 C : UV210nm : 1; Cholesterol (5.6 g) 2; Stigmasterol (5.9 g) 3; Campesterol 4; tosterol R= AP R 1; 3C 3; 3C 2; 3C 3C 4; ACALAI TESQUE, IC AP-1026 VI. Technical otes CSMSIL Application Data Mobile phase: Methanol/ 2 = 30/70 AP Methanol/ 2 = 50/50 Methanol/ 2 = 80/20 Flow rate: : 30 C : UV254nm AP VII. Index : ; Phthalonitrile (0.3 g) ; Isophthalonitrile (3.0 g) ; Terephthalonitrile (0.15 g) ACALAI TESQUE, IC AP

6 Applications Attention CSMSIL Application Data Mobile phase: Methanol/ 2 = 95/5 AP Methanol/ 2 = 90/10 Methanol/ 2 = 90/10 Flow rate: : 30 C : UV295nm : CSMSIL Application Data Mobile phase: Methanol/ 2 = 70/30 Flow rate: : 30 C : UV280nm : 1; Capsaicin (1.0 g) 2; -Vanillylnonanamide (0.5 g) 3C R 1 R 2 3C 1. Methanol is recommended as a mobile phase for CSMSIL PYE column. Acetonitrile is not recommended because it has - 2. The stationary phase of CSMSIL PYE, pyrenylethyl group, has a large UV absorption. When the stationary phase detaches from silica gel and elutes, even a slight quantity can be detected and causes baseline noise. In such a case, wash the column with tetrahydrofuran. Detachment of a small amount of the stationary phase does not deteriorate a column s separation ability. 3. CSMSIL PYE column is not suitable for gradient analysis. rdering Information Capsaicin -Vanillylnonanamide CSMSIL Packed Column 3C 1.0 x x x AP 4.6 x x x x AP ACALAI TESQUE, IC AP-1073 CSMSIL Guard Column ACALAI TESQUE, IC AP x x x x I. PLC Columns II. UPLC Columns III. Preparative IV. Related Products V. Applications VI. Technical otes VII. Index Packing Materials 27

7 I. PLC Columns II. UPLC Columns III. Preparative Packing Materials Excellent separation for structural isomers Selectivity for Dipole-dipole Interactions 1,8-dinitronaphthalene because of the strong dipole formed by the two nitro groups positioned on the same side of naphthalene. Comparison of Separation Property Mobile phase: PE Methanol / 2 = 70/30 PYE Methanol / 2 = 90/10 C 18 -MS-II Methanol / 2 = 80/20 Flow rate: : 30 C : UV254nm : 1; 1,8-Dinitronaphthalene 2; 1,5-Dinitronaphthalene 3; aphthalene 4; 1-Methylnaphthalene 5; 1,5-Dimethylnaphthalene C 18- MS-II ACALAI TESQUE, IC AP-1074 IV. Related Products Attention from silica gel and elutes, even a slight quantity can be detected and causes baseline noise. In such a case, wash the column with tetrahydrofuran. Detachment of a small amount of the stationary phase does not deteriorate a column s separation ability. 3. V. Applications VI. Technical otes rdering Information Analytical / Preparative Column 1.0 x x x x x x x x x x x VII. Index 28

Inertsil ODS-EP Technical Information

Inertsil ODS-EP Technical Information Technical Information Advantages of The selectivity is completely different from those of conventional columns such as ODS column due to its specific polar group in the stationary phase. Durability can