Advanced liquid chromatographic instrumentation for preparative separations ranging from mg to gram scale has been combined into one laboratory. Together with new analytical screening capabilities, the benefits include more efficient work flows and leaner preparative purification.
Fig.1 Semi-preparative LC/UV/MS at
SP Process Development
SP Process Development can assist in chromatographic purification of materials of up to ca 300mg by semi-preparative LC/UV/MS and up to ca 10g by preparative LC/UV.
We offer both reversed phase and normal phase LC preparative separations. Reverse phase separations are performed on C18 or C8 column material, typically eluted with gradients of an aqueous buffer in methanol or acetonitrile. We also perform normal phase LC separations over silica columns were the mobile phase consists of organic solvent mixtures such as Dichloromethane/Methanol or Heptane/Ethyl acetate. Flash silica chromatography on our ISCO system is also an option.
Examples of separations we can perform
• Isolation of minor impurities - eg an unknown impurity appearing
during a stability study
• Complex separations - eg purification of a major Component
from a synthetic mixture
• Chiral separations
For chiral applications we have a broad range of chiral phases available, with sizes ranging from analytical columns to preparative scale columns, eg different Chiralcel and LUX columns.
With an HPLC evaluation system we have the possibility of screening up to 6 different columns for easy identification of an appropriate chiral phase. For optimising a separation, three solvents systems can also be screened simultaneously. Solvent systems typically applied in chiral column screening are gradients with Ethanol, Isopropyl alcohol or Ethanol/Methanol 50:50 in Heptane.
Examples of problem solving packages SP Process Development offer where preparative separation form a part are:
• Characterisation of impurity
Isolation of an impurity from a product by preparative chromatography, followed
by complete structure elucidation by NMR and LC/MS/MS of the impurity.
• Absolut configuration determination of enantiomer
Chiral preparative separation of a racemate, followed by crystallisation and absolute
configuration determination by single X-ray crystallography of the enantiomers.