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Application Note P6.0 SPE Extraction using SiliaPrep ...€¦ · SPE Extraction using SiliaPrep...
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Si [email protected], www.SiliCycle.com Tel.: 1 418.874.0054, Toll-free: 1 877.SILICYCLE (North America only) SiliaPrep ™ Application Note P6.0 SPE Extraction using Silia Prep Fluorochrom SiliaPrep Fluorochrom (or Si-FCM) is a fluorinated sorbent particularly useful for the separation of fluorine containing molecules from non-fluorous ones. This new technique is slowly gaining acceptance in the scien- tific community mostly for it’s applications in SPE and HPLC. The applications of these types of sorbents are not limited to fluorous compounds and they may also include chromatographic separations of non-fluo- rinated molecules, just like a regular reversed-phase would do, but with a different selectivity. SiliaPrep Fluorochrom presents the highest level of fluorine available on the market and has a proprietary structure. SiliaPrep Fluorochrom silica gel will selectively retain fluorous compounds while non-fluorous ones will be directly eluted out of the cartridge, regardless of the polarity. Using these cartridges, you will be able to get a quick and easy separation of fluorous compounds from different reactions mixtures. This separation method can be applied either for scavengers, protecting groups, tags as well as reagents fluorine content. This method utilizes an easy two-step elution process based on solvent selectivity (fluorophobic and fluo- rophilic solvents). This is a typical demonstration using dyes to show the procedure using SPE Cartridges packed with SiliaPrep Fluorochrom silica gel (in blue is an organic dye and in yellow a fluorous dye). Typical loading capacity for these cartridges is 5-15% of the silica bed weight. EXTRACTION PROCEDURE SPE Cartridge type: PN Cartridge Size Typical Capacity SPE-R63730B-01B 0.05 g/1 mL 2.5-7.5 mg SPE-R63730B-01C 0.10 g/1 mL 5.0-15.0 mg SPE-R63730B-03G 0.20 g/3 mL 10.0-30.0 mg SPE-R63730B-03P 0.50 g/3 mL 25.0-75.0 mg SPE-R63730B-06P 0.50 g/6 mL SPE-R63730B-06S 1.00 g/6 mL 50.0-150.0 mg SPE-R63730B-06U 2.00 g/6 mL 100.0-300.0 mg SPE-R63730B-12U 2.00 g/12 mL SPE-R63730B-20X 5.00 g/20 mL 250.0-750 mg Note: Other cartridge size and silica weight available on request. Sample pre-treatment: • Dissolve the sample in the minimum volume of DMF possible SPE extraction using SiliaPrep Fluorochrom: • Cartridge conditioning step Wash the cartridge with a minimum volume of solvent to remove impurities coming from the cartridge moulding step (oil). Discard collected fraction. - Solvent: DMF - Volume: < 1 column volume
Transcript of Application Note P6.0 SPE Extraction using SiliaPrep ...€¦ · SPE Extraction using SiliaPrep...
Si
[email protected], www.SiliCycle.comTel.: 1 418.874.0054, Toll-free: 1 877.SILICYCLE (North America only)
SiliaPrep™
Application Note P6.0 SPE Extraction using SiliaPrep Fluorochrom
SiliaPrep Fluorochrom (or Si-FCM) is a fluorinated sorbent particularly useful for the separation of fluorine containing molecules from non-fluorous ones. This new technique is slowly gaining acceptance in the scien-tific community mostly for it’s applications in SPE and HPLC. The applications of these types of sorbents are not limited to fluorous compounds and they may also include chromatographic separations of non-fluo-rinated molecules, just like a regular reversed-phase would do, but with a different selectivity. SiliaPrep Fluorochrom presents the highest level of fluorine available on the market and has a proprietary structure.
SiliaPrep Fluorochrom silica gel will selectively retain fluorous compounds while non-fluorous ones will be directly eluted out of the cartridge, regardless of the polarity. Using these cartridges, you will be able to get a quick and easy separation of fluorous compounds from different reactions mixtures. This separation method can be applied either for scavengers, protecting groups, tags as well as reagents fluorine content. This method utilizes an easy two-step elution process based on solvent selectivity (fluorophobic and fluo-rophilic solvents).
This is a typical demonstration using dyes to show the procedure using SPE Cartridges packed with SiliaPrep Fluorochrom silica gel (in blue is an organic dye and in yellow a fluorous dye). Typical loading capacity for these cartridges is 5-15% of the silica bed weight.
EXTRACTION PROCEDURE
SPE Cartridge type:
PN Cartridge Size Typical Capacity
SPE-R63730B-01B 0.05 g/1 mL 2.5-7.5 mg
SPE-R63730B-01C 0.10 g/1 mL 5.0-15.0 mg
SPE-R63730B-03G 0.20 g/3 mL 10.0-30.0 mg
SPE-R63730B-03P 0.50 g/3 mL25.0-75.0 mg
SPE-R63730B-06P 0.50 g/6 mL
SPE-R63730B-06S 1.00 g/6 mL 50.0-150.0 mg
SPE-R63730B-06U 2.00 g/6 mL100.0-300.0 mg
SPE-R63730B-12U 2.00 g/12 mL
SPE-R63730B-20X 5.00 g/20 mL 250.0-750 mg
Note: Other cartridge size and silica weight available on request.
Sample pre-treatment: • Dissolve the sample in the minimum volume of DMF possible
SPE extraction using SiliaPrep Fluorochrom:
• Cartridge conditioning step
Wash the cartridge with a minimum volume of solvent to remove impurities coming from the cartridge moulding step (oil). Discard collected fraction.
- Solvent: DMF - Volume: < 1 column volume
Si
[email protected], www.SiliCycle.comTel.: 1 418.874.0054, Toll-free: 1 877.SILICYCLE (North America only)
SiliaPrep™
SPE extraction using SiliaPrep Fluorochrom:
• Column equilibration step Wash the cartridge with a “fluorophobic” solvent for better reproducibility. - Solvent: 80/20 MeOH/H2O - Volume: 1-2 column volume - Flow rate: 2-4 mL/min
• Sample loading - Load directly the prepared sample on the top of the cartridge under vacuum (if using an SPE vacuum manifold or either an SPE vacuum adaptor) or positive pressure. - Flow rate: same rate as the cartridge volume 1 mL SPE Cartridge : 1 mL/min 3 mL SPE Cartridge : 3 mL/min 6 mL SPE Cartridge : 6 mL/min, etc.
• Non-Fluorous compounds elution step (Fluorophobic elution) Elute non-fluorous compounds using a “fluorophobic” solvent.
- Solvent: 80/20 MeOH/H2O - Volume: 2-3 column volume - Flow rate: 1-2 mL/min
Note: Water content is very important to prevent the chance of fluorous breakthrough. Acetonitrile and ethanol mixed with at least 20% of water can also be used as “fluorophobic” solvents.
• Fluorous compounds elution step (Fluorophilic elution) Fluorinated compounds are eluted using methanol.
- Solvent: Methanol - Volume: 2-3 column volume - Flow rate: 1 mL/min
Note: Acetonitrile can also be used as “fluorophilic” solvent for the elution. More “fluorophilic” solvents like THF and Acetone can be employed as well.
• Regeneration of the SiliaBond Fluorochrom phase To regenerate the SiliaBond Fluorochrom SPE cartridge, wash the stationary phase with appropriate solvent, then dry the cartridge (air dry sufficient)
- Solvent: THF or Acetone - Volume: 1-2 column volume
Si
[email protected], www.SiliCycle.comTel.: 1 418.874.0054, Toll-free: 1 877.SILICYCLE (North America only)
SiliaPrep™
SPE Troubleshooting:
• If your fluorinated compounds is not well retained, try to minimize solvent loading, change SPE cartridge size (sorbent weight), change sample dissolving solvent and/or increase the water content in the equilibrium step (50/50 Methanol/H2O).
