24 Hours To Pure Sample From Sample Receipt

ASMS 2011, Salt Lake City, UT, USA, 23-27 June 2011, Mark Bayliss, Joseph Simpkins, Stephane Murphy, Martin Fuhr, Utz-Peter Jagusch, Josephine Archinal, Stefan Oberbörsch

Support of Medicinal Chemistry, Compound Collection and our Synthetic Chemists requires our laboratories to deliver purified, confirmed chemistries for downstream activities. Historically sample turnaround times were both variable and often longer than all departments were happy with. Using both internal and external expertize, the entire end-to-end workflow has been revisited, refined and automated with screening results and purified materials now being turned around in 24 hours. This presentation focuses on the challenges there were faced and how these were practically solved and the automation environment that was required to deliver to the project needs.


Synthesis samples from both manual and automated synthesis environments are screened using a combination of low resolution Agilent Single Quadrupole and Agilent 1290 Tof instruments. Purification is accomplished using a mixture of both Waters and Agilent MS directed auto-purification systems. Purified substances are then analyzed for target validation, sample purity and sample homogeneity using a number of Waters uPLC/MS Single Quadrupole instruments. Data are all analyzed using an automated client-server software environment from Virscidian Inc.

Preliminary data

The system has now been in operation since summer 2010 and been used in over 50,000 sample analyses. At each stage the results are assessed in the same software application environment against specific evaluation criteria that are appropriate to the stage of the sample. A number of common evaluation criteria across all stages include accuracy of data processing across all detectors but most importantly for the detector(s) used to confirm Area% of the target. Additionally accuracy of target determination and accuracy of the automated results interpretation are also critical. Our preliminary data suggests that once an optimal data processing method is generated for an instrument, that no additional reprocessing of results is required. Indeed where automated results interpretation failure exists, the sample quality is typically not appropriate for further assessment. Indeed the level of results review has dramatically reduced from 100% review of all samples across all phases, to just the samples that are flagged for review and a general low percentage review of the remaining results for quality control purposes. During the presentation, we discuss the challenges that were faced in implementing such a system, an overview of the system that is currently in production usage and expectations for future enhancements to allow for additional automation improvements.

Novel aspect

Cross platform integration and automation for a seamless high accuracy system of purified compound production in 24 hours.