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SiliaChrom®- CHIRAL HPLC Columns

SiliaChrom Chiral coated polysaccharide stationary phases are made with a spherical high quality silica support physically coated with a polymeric chiral selector such as amylose or cellulose derivatives. Due to the coated nature of these supports, solvents should be carefully selected for the normal phase conditions.

SiliaChrom Chiral Cellulose T-DPC: Cellulose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L40). SiliaChrom Chiral Cellulose T-DPC is the most popular phase used for chiral separation of alkaloids, tropines, amines and beta blockers.

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SiliaChrom Chiral Cellulose T-MB
: Cellulose tris-(4-methylbenzoate) coated on a spherical silica support. SiliaChrom Chiral Cellulose T-MB is used for chiral separation of aryl methyl esters and aryl methoxy esters.

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SiliaChrom Chiral Amylose T-DPC
: Amylose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L51). SiliaChrom Chiral Amylose T-DPC is used for chiral separation of alkaloids, tropines, amines and beta blockers

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Main characteristics

  • Mechanically strong (longer lifetime)
  • High loadability
  • High selectivity (high efficiency and resolution)
  • Unique coating method (proprietary)
  • Easy to scale-up

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Operating restrictions for all SiliaChrom chiral phases

SiliaChrom Chiral Cellulose T-DPC, Cellulose T-MB, Amylose T-DPC
 

250 x 4,6 mm
Analytical column

250 x 10 mm
Semi-prep. column

250 x 20 mm
Semi-prep. column

Flow direction As indicated on the column label
Flow rate1

~ 1 mL/min
Do not exceed 1,5mL/min

~ 5 mL/min
Do not exceed 7mL/min

~ 18 mL/min
Do not exceed 25mL/min

Pressure limits2 < 30 Bar (430 psi)3 for maximum lifetime and do not exceed 50 Bar (~700 psi)
Temperature 0 to 40°C 0 to 40°C 0 to 40°C

1 The maximum flow rate depends on the mobile phase viscosity (mobile phase composition), and should be adjusted in accordance with the pressure upper's limit (50 Bar).

2 The back pressure value that should be taken into account is the one generated by the column itself. This value is measured by calculating the difference between the pressure of (LC system + column) and the pressureof the LC system free of the column.

3 Ideal value for maximum column life, but stable up to 50 Bar.

SiliaChrom Chiral Cellulose T-DPC, Cellulose T-MB, Amylose T-DPC
Examples 250 x 4,6 mm
Analytical column
250 x 10 mm
Semi-prep. column
250 x 20 mm
Semi-prep. column
Alkane/Alcohol (90/10) 1,0 to 1,5 mL/min 5 to 7 mL/min 18 to 25 mL/min
100% EtOH ~ 0,5 mL/min 2 to 3 mL/min 5 to 8 mL/min
100% 2-propanol ~ 0,3 mL/min ~ 1 mL/min 3 to 5 mL/min

 

Operating procedure of SiliaChrom Chiral Cellulose T-DPC and SiliaChrom Chiral Cellulose T-MB

Mobile phases:

SiliaChrom Chiral Cellulose T-DPC and SiliaChrom Chiral Cellulose T-MB
SiliaChrom OD Alkane1/2-propanol2 Alkane1/EtOH2 Alkane1/MTBE Alkane1/MeOH3 MeOH4+5
250 x 4,6 mm 100/0 to 0/100 100/0 to 0/100 100/0 to 50/50 100/0 to 0/100

0 to 100%
EtOH or IPA
in MeOH

250 x 10 mm 100/0 to 0/100 100/0 to 0/100 100/0 to 50/50 100/0 to 0/100
250 x 20 mm 100/0 to 0/100 100/0 to 0/100 100/0 to 50/50 100/0 to 0/100

1Alkane: n-hexane, iso-hexane or n-heptane. Some small selectivity differences may sometimes be found.

2The retention is generally shorter with Ethanol than with 2-propanol.
  The retention is generally shorter with a higher alcohol content.
  The use of other alcohols such as 1-propanol, 1-BuOH, 2-BuOH ... is possible, buth effectiveness cannot be guaranteed.

3 Due to limited miscibility of MeOH in Alkane, it is necessary to add an appropriate volume of EtOH together with MeOH in order to obtain an homogeneous solvent mixture. A maximum of 5% MeOH in n-hexane may be used without adding EtOH.

4 Ideal starting conditions: MeOH/EtOH 50:50 (v/v) when alcohol mixtures are required.

5 The use of polar solvents as 100% methanol is possible with SiliaChrom Chiral Cellulose T-DPC column. Nevertheless, once the column is transfered to a polar mode it should be dedicated to this specific application.
To safely transfer the column from hexane to methanol it is strongly recommended to use 100% 2-propanol as a transition mobile phase at a low flow rate (high viscosity of 2-propanol).

Modifiers:
For basic or acidic samples, it is necessary to add a modifier into the mobile phase in order to achieve the chiral separation: 6 for primary amines mainly and 7 for primary amino alcohols mainly.

SiliaChrom Chiral Cellulose T-DPC and SiliaChrom Chiral Cellulose T-MB
Basic samples require basic modifiers DEA, Butyl amine6, EtOH amine7 <0,5%, typically 0,1%
Acidic samples require acidic modifiers TFA, CH3COOH, HCOOH (OJ) <0,5%, typically 0,1%

 

Operating procedure of SiliaChrom Chiral Amylose T-DPC

Mobile phases:

SiliaChrom Chiral Amylose T-DPC
SiliaChrom AD

Alkane1/ 2-propanol2

Alkane1/EtOH2 Alkane1/MeOH3 MeOH4+5 CH3CN5+6
250 x 4,6 mm 100/0 to 0/100

100/0 to 85/15
and
40/60 to 0/100

100/0 to 85/15
and
40/60 to 0/100

0 to 100%
EtOH or IPA
in MeOH
0-15%
CH3CN
in MeOH

0 to 100%
EtOH or IPA
in MeOH
0-15% MeOH
or EtOH7
in CH3CN

250 x 10 mm
250 x 20 mm

1 Alkane: n-hexane, iso-hexane or n-heptane. Some small selectivity differences may sometimes be found.

2 The range Hexane/EtOH 85/15 ~ 40/60 may adversely affect baseline stability dur to polymer leakage.
To safely transfer the column from 15% EtOH to 60% EtOH, it is strongly recommended to use 100% 2-propanol as a transition mobile phase at a low flow rate (high viscosity of 2-propanol).
The retention is generally shorter with Ethanol than with 2-propanol.
The retention is generally shorter with a higher alcohol content.
The use of other alcohols such as 1-propanol, 1-BuOH, 2-BuOH ... is possible, buth effectiveness cannot be guaranteed. Do not use mobile phases containing more than 15% of these alcohols.

3 Due to the limited miscibility of MeOH in Alkane, it is necessary to add an appropriate volume of EtOH together with MeOH in order to obtain an homogeneous solvent mixture. A maximum of 5% MeOH in n-hexane only may used without adding EtOH.

4 Ideal starting conditions: MeOH/EtOH 50:50 (v/v) when alcohol mixtures are required.

5 The use of polar solvents as 100% methanol or 100% acetonitrile is possible with SiliaChrom Chiral Amylose T-DPC column. Nevertheless, once the column is transfered to a polar mode it should be dedicated to this specific application.
To safely transfer the column from n-hexane to methanol or acetonitrile or between different polar solvents, it is strongly recommended to use 100% 2-propanol as a transition mobile phase at a low flow rate (high viscosity of 2-propanol).

6 More than 15% of alcohol other than 2-propanol, in acetonitrile may destroy the column. Compatibility of such mixtures with the chiral stationary phase cannot be guaranteed.

7 The use of other alcohols such as 1-propanol, 1-BuOH, 2-BuOH ... is possible, buth effectiveness  cannot be guaranteed. Do not use mobile phases containing more than 15% of these alcohols.

Modifiers:

For basic or acidic samples, it is necessary to add a modifier into the mobile phase in order to achieve the chiral separation: 8 for primary amines mainly and 9 for primary amino alcohols mainly.

SiliaChrom Chiral Amylose T-DPC
Basic samples require basic modifiers DEA, Butyl amine8, EtOH amine9 <0,5%, typically 0,1%
Acidic samples require acidic modifiers TFA, CH3COOH, HCOOH (OJ) <0,5%, typically 0,1%

 

Application Note

SiliaChrom Chiral Amylose T-DPC - Enantiomeric Separation of L & D-val-PMB

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  1. SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom Chiral Cellulose T-MB: Cellulose tris-(4-methylbenzoate) coated on a spherical silica support. SiliaChrom Chiral Cellulose T-MB is used for chiral separation of aryl methyl esters and aryl methoxy esters.

  2. SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Cellulose T-DPC

    SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Cellulose T-DPC

    Cellulose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L40). SiliaChrom Chiral Cellulose T-DPC is the most popular phase used for chiral separation of alkaloids, tropines, amines and beta blockers.

  3. SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Amylose T-DPC

    SiliaChrom® Semi-Preparative HPLC Columns CHIRAL Amylose T-DPC

    Amylose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L51). SiliaChrom Chiral Amylose T-DPC is used for chiral separation of alkaloids, tropines, amines and beta blockers.

  4. SiliaChrom® Preparative HPLC Columns CHIRAL Cellulose T-DPC

    SiliaChrom® Preparative HPLC Columns CHIRAL Cellulose T-DPC

    Cellulose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L40). SiliaChrom Chiral Cellulose T-DPC is the most popular phase used for chiral separation of alkaloids, tropines, amines and beta blockers.

  5. SiliaChrom® Preparative HPLC Columns CHIRAL Amylose T-DPC

    SiliaChrom® Preparative HPLC Columns CHIRAL Amylose T-DPC

    Amylose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L51). SiliaChrom Chiral Amylose T-DPC is used for chiral separation of alkaloids, tropines, amines and beta blockers.

  6. SiliaChrom® HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom® HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom Chiral Cellulose T-MB: Cellulose tris-(4-methylbenzoate) coated on a spherical silica support. SiliaChrom Chiral Cellulose T-MB is used for chiral separation of aryl methyl esters and aryl methoxy esters.

  7. SiliaChrom® Analytical HPLC Columns CHIRAL Cellulose T-DPC

    SiliaChrom® Analytical HPLC Columns CHIRAL Cellulose T-DPC

    Cellulose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L40). SiliaChrom Chiral Cellulose T-DPC is the most popular phase used for chiral separation of alkaloids, tropines, amines and beta blockers.

  8. SiliaChrom® Analytical HPLC Columns CHIRAL Amylose T-DPC

    SiliaChrom® Analytical HPLC Columns CHIRAL Amylose T-DPC

    Amylose tris-(3,5-dimethylphenylcarbamate) coated on a spherical silica support (USP Code L51). SiliaChrom Chiral Amylose T-DPC is used for chiral separation of alkaloids, tropines, amines and beta blockers.

  9. SiliaChrom® Analytical HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom® Analytical HPLC Columns CHIRAL Cellulose T-MB

    SiliaChrom Chiral Cellulose T-MB: Cellulose tris-(4-methylbenzoate) coated on a spherical silica support. SiliaChrom Chiral Cellulose T-MB is used for chiral separation of aryl methyl esters and aryl methoxy esters.

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