Chromatography focus on
The Chromatographic Society Spring Symposium 2011 11-12th May 2011, Norvartis Institute of Biomedical Research, Horsham, UK Nicola Gray, Pharmaceuticle Science Division, Kings College London. Email
nicola.gray@
kcl.ac.uk
The Chromatography Society recently held their annual Spring Symposium at the Norvartis Institute of Biomedical Research, Horsham, UK. The theme of the meeting was Advances in Separation Science, principally focused on small molecule analysis in pharmaceutical drug discovery. The agenda for the one-and-a-half day event included a host of international speakers from academia and industry alongside vendor presentations with significant exhibition and networking time. An encouraging number of delegates were attracted to this meeting across the spectrum with an interest in the latest developments in separation science.
The Scientific Programme
The meeting started with a warm welcome from Ian Clemens, Director GDC Norvartis, Alan Handley chaired the first session after thanking attendees, sponsors and organisers of the meeting.
The first keynote speaker was Wolfgang Lindner from the University of Vienna who spoke about ‘Enantiomer Separations with Chiral Ion Exchangers, a Unique Class of Chiral Columns’. He described the development of highly selective ion-exchanger chiral phases based quinine and quinidine as selectors immobilised onto the stationary phase support. The application of these columns was exemplified in both RPLC and SFC, illustrating enantiomer separation of primary amines and acids on an analytical and preparative scale.
The increasing popularity of supercritical fluid chromatography (SFC) was resonant throughout this meeting, with the second lecture presented by Jeremy Glennon from University College Cork, Ireland. His talk, entitled ‘Recent Progress in Supercritical Functionalisation and Superficially Porous Particles’, focused on his
research into novel stationary phases and the use of SC-CO2 in the preparation of functionalised silica phases. He also highlighted his work into on-chip separation devices and the preparation of nanomaterials for ion chromatography on a chip.
Andy Aubin from Waters spoke on behalf of the principal sponsors of this event on ‘Harnessing the Power of sub-2 um Chromatographic Particles in Supercritical Fluid Chromatography’. He discussed the new Waters Acquity UPSFC system, recently launched as an alternative to PPLC, which can utilise sub-2 micron particles. He gave an account of the development of the system and investigations, highlighting the benefits of increased sensitivity, resolution and speed sub-2 um particles realised in HPLC. Andy also highlighted that peak efficiencies may not be representative when measured using isobaric conditions to construct van Deemter plots, and suggests using isopycnic conditions to overcome the effect of changes in mobile phase solvating strength.
Dr Pilar Franco from Chiral Technologies, France, opened the vendor session with ‘Supercritical Fluid Chromatography Screening Strategies for Chiral Separations’, proposing that a primary chiral screen should utilise the IA, IB, IC and ID columns (all immobilised selectors) which are compatible with a much greater range of solvents than the older non-covalent bonded materials. A secondary screen would include AD-H, AS-H, AY-H and the ‘O’ equivalents.
D Berger from Chemputeam, Switzerland, followed on, speaking about Aurora SFC and the difficulties associated with pumping low percentage organic with current SFC pumping technology, in particular from a sensitivity point of view due to system noise. The merits of SuperSep instrumentation were also highlighted for recycling CO2 in prep scale separations.
Tony Taylor from Crawford Scientific then introduced Poroshell, Agilent’s first fused core particle. He highlighted the benefits of such superficially porous particles and also proposed that efficiency per unit pressure (N per bar) was a good way to assess a column and highlighted this by presenting examples with coupled columns.
A short tea break then quickly sees us into the final session of the day from invited lecturers on Analytical Support of Drug Discovery. Following an introduction from Dr Jeff Hearm, MSD, Dr John Langley from the University of Southampton spoke of ‘Achiral SFC-MS and Small Molecules – An Analyst’s View’. John discussed the use of a modifier to improve tailing peaks of certain compounds and highlighted the need to T in a make-up flow of liquid prior to the source capillary to prevent freezing of the capillary due to CO2, typically 5 mM ammonium acetate is used for this.
Novartis, Horsham
He also described an unusual phenomenon whereby ionisation of analytes was observed with the capillary voltage turned off in both APCI and ESI modes, thought to be due to ‘sonic spray’ process.
To conclude the first day, Brian Everatt from Novartis gave us an enthusiastic account of ‘Remote Open Access – The Lab2LabTM Advantage’, highlighting Norvartis’ novel approach to open allowing chemists to run their own samples without having to even set foot into an analytical laboratory. This automated sample delivery and analysis system for and open access chemist use. Samples input a small amount of data on a terminal linked to the Lab2Lab system. The sample vial is placed in a holder and placed into the loading unit, which is moved though tubing via compressed air to a router. The router is intelligent enough to know which systems are idle and sent the sample to an appropriate instrument for analysis. The system is scalable to any lab size.
The second day of the event started with an incredibly moving eulogy to the late Uwe Neue from Pam Iraneta (Waters), a close colleague and friend to Uwe. She highlighted the successes and huge contributions the great chromatographer had over his career, 130 publications and instilled the sense of enjoyment that Uwe gained from sharing his knowledge with those keen to learn from him.
This apt introduction for the following session, chaired by John Lough, enables us to see the benefits of collaborations between active research groups. Professor Peter Myers began with his innovative HPLC on a Compact Disc. Channels are etched into a compact disc, and capillary tubes are packed with silica and placed in the grooves. The sample in place in a chamber and is held behind a wax coated bead which is melted by a standard CD player laser and allows introduction of the sample. The sample is moved through the column using the centrifugal flow of the spinning CD and is detected using the standard CD laser detection, which identifies compounds leaving the column as ‘errors’. These error codes in the bit pattern are converted into chromatogram peaks and show the separation.
James Heaton (King’s College London) followed on with an insightful presentation on his Investigation into the effect and utility of temperature in ultra high performance liquid chromatography, highlighting the merits and challenges associated with high temperature LC. He appropriately illustrated the importance of using a mobile phase pre-heater to prevent thermal mismatch, a phenomenon duly noted by Uwe who proceeded invent the curved pre-heater Waters use today. James investigated the effect of different types of thermostat on column efficiency, including forced air (Polaratherm) and still air (Acquity) variants. For efficient heat transfer in and out of the column, a large surface area to column volume ratio is
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