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that have been included here, again reducing the analysis, evaporation and overall process time for completion of the related sample.
The management of the revised process workflow has been achieved through standardization of the two preparative HPLC instruments used. To ensure each purification is achieved through a single injection, both systems have a 20 ml sample loop, allowing flexibility to inject >5 ml volume if required. Each of these systems utilises a 5 µm 50 x 150 mm column sufficient for all purifications up to approximately 1 g of crude material. Typically, most samples purified range between 100 – 500 mg and could easily be accommodated. These columns were chosen for their robustness, efficiency and ability to sustain both acidic and basic separations. To ensure that each individual sample could be purified accordingly and without delay, each instrument was provisionally dedicated to either acidic or basic modifier. However, the ability to switch modifiers through these columns allowed the flexibility of using both systems simultaneously with the same modifier. This allowed the service to accommodate larger workloads when required. The availability and standardisation of these HPLC systems provided a contingency plan to support the service with
back up in the event of failure of one of the instruments. In addition, this also helped to maintain continuity for the individuals providing cover in times of absence.
Conclusions This revised process workflow has been functional within the department for over 18 months and has proved to continually support customer requirements, with an average of 80 final compounds per month generated from synthetic chemistry. As the capacity available in the service allows for 160/month, this can comfortably accommodate increases in demand whilst maintaining the efficiency and turnaround time in line with the customer expectations. This improvement project has been modeled on a prep HPLC purification platform but the flexibility in capacity allows for further adaptations. As part of Continuous Improvement, the service has progressed to the incorporation of normal phase chromatography in line with changing customer demands. To accommodate both 12 g and 40 g silica columns, the process workflow is maintained utilising 1 & 2 purification slots (30 minutes) per run respectively. The timeframe to complete these purifications can vary between samples but this time can be redeemed through the evaporation of purely organic solvent.
Specially Engineered Chromatography Systems
Cambridge Scientific Instruments Ltd are pleased to offer full gas chromatography systems specially engineered to the customer’s exact needs. With over 30 years experience in the industry and by listening to and understanding customers problems CSI are able to design and produce one off custom solutions to their analytical needs. Using the versatile 200 series GC as the base CSI can offer a wide range of customisation options to meet a customer’s requirements.
Installed Systems include
• Alternator Gas Analyser • Biofuel Analyser • Low power GC for mobile laboratories • Automated material analysis for solvent breakthrough • Continuous online whiskey Process monitor • Multiple selective detection systems
For further information on what CSI can offer please visit
www.camsci.co.uk/secs.html ASTM Approves Column Set
Labs testing ethanol-containing finished gasolines now have a better alternative to TCEP columns. At its recent meeting, the ASTMD02 Committee announced a revision to method D3606 which now includes the D3606 column set from Restek. This column set separates benzene from ethanol completely and much more reliably than TCEP columns, resulting in more accurate quantification and tighter process control. Since a third column is not required, use of this column set simplifies installation and analysis. Additionally, all D3606 column sets are tested for method applicability and have higher thermal stability than TCEP columns, resulting in longer column lifetimes.
For further information visit
www.astm.org
Offering this technique as part of the service has proved successful and encourages the use for key intermediate purifications alongside final compounds if spare capacity is available. It is envisaged that this revised process will continually improve through innovative thinking and customer feedback, critically assessing the ability to meet alternative or additional requirements.
Through adaptation of the working practices and customer collaboration a valuable reduction in turnaround time from 21 hours to 4 hours has been achieved. In addition, the alternative evaporation techniques have reduced the overall energy costs to 25% of the pre-improvement cost per individual sample. Consequently, the successful outcome of this project demonstrates the benefit of observing processes from a Lean Sigma perspective to implement the most appropriate, efficient and effective improvement strategies.
References
1. C. Johnstone & J. Kihlberg et al., Making medicinal chemistry more effective - application of Lean Sigma to improve processes, speed and quality, Drug Discovery Today 14 (2009), pp.598-604 2.
www.lean.org,
www.isixsigma.com,
www.sixsigmainstitute.com
3.http://
www.isixsigma.com/
index.php?option=com_k2&vie w=item&id=1013:sipoc-diagram&Itemid=219 4.
http://www.valuestreamguru.com/?p=123
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