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Meeting Reports
Chromatographic Society Meetings Round-Up “Current Method Development Strategies in Separation Science” Chromatographic Society Spring Symposium, 19th and 20th May 2010, Merck Sharp and Dohme, Hoddesdon,Herts. by E A Adlard
The topic of this meeting was “Current Method Development Strategies in Separation Science” although a more accurate title would have been “Current Method Development Strategies in HPLC in the Pharmaceutical Industry” since this was the theme of all the papers except for one on SFC. To one who has been in the field for a long time and can now afford the luxury of an overview the current situation in HPLC seems to bear a resemblance to GC in the days of packed columns when there were hundreds of stationary phases available, many of them giving identical separation. This dilemma was rationalised in GC with the development of high efficiency silica capillary columns and to a certain extent HPLC is following the same road with the development of uHPLC. However, HPLC has many more parameters that can be changed than GC so that arriving at optimum separation is a much more complicated process.
The opening talk was by Dr Chris Welch on “Chiral Chromatographic Method Development”. Chiral stationary phases (CSP) may be extremely expensive to prepare but Dr Welch has developed methods of microscale, multiparallel method development with a “coffee-break cycle time” (scientific) evaluation requiring only a few milligrams of material. This allows more CSP including experimental ones to be evaluated, thus ensuring that it is the very best chiral separation that progresses towards preparative work. Also, loading studies to optimise up-scale throughput may be carried out on the microscale systems.
The next keynote lecture was given by Dr John Dolan, well-known for his articles on various aspects of liquid chromatography in LC- GC. He emphasised that many of the columns on the market from different suppliers and different names were in fact very similar in their separation abilities. This in itself, is not necessarily a bad thing since it means that equivalent replacements are available if a particular supplier ceases to market a given column but orthogonal separations require columns with a widely different separation
capabilities as possible. The use of test probes enabled an “F factor” (a fitting similarity) to be obtained. Values of F less than 3 means that columns are essentially the same and those with a factor greater than 60 are very different. Dr Dolan recommended consultation of the RQRI (Product Quality Research Institute) database in which 476 RP phases were
compared. This should allow identification of similar and different columns to allow the orthogonal separation of difficult pairs. There was no mention of time in this argument since it might be quicker to run mixtures quickly on two different columns rather than seek good separation on one column in a longer net time.
The next session consisted of three presentations, the first of which was by Dr Tom van de Goor of Agilent (the principal sponsoring company of the meeting). Dr van de Goor pointed out that method development is an ongoing task in many analytical labs especially those involved in the development of new drugs and regulatory requirements often result in demands for better sensitivity, resolution and speed of analysis. Method development is a laborious and time –consuming task and automated method development reduces the time required and permit screening of many more separation conditions.When an optimised method has been developed in one location it may need to be transferred to other labs using different instruments. De Goor proposed a new approach that simplifies transfer from uHPLC to HPLC and vice versa without changes to the method or instrument modification.
This was followed by a paper presented by Tony Edge of Thermo Fisher on the optimisation of SPE clean-up before final separation by HPLC and mass spectrometric detection. Examples were given of how this approach could be used for the analysis of a range of pharmaceutical compounds in biological matrices. The final two talks of the day were by speakers on the analysis of drugs and intermediates for genotoxic impuritites. A number of groups and organic fragments had been recognised as potentially genotoxic and these were identified as either occurring in intermediates or as impurities in final products by both GC and HPLC. It is to be hoped that the fact that both these papers were by speakers from the
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