omation mbers - Society for Laboratory Automation and Screening

8:00 am Wednesday, February 4 HT Chemistry – Analytical Room B3
Götz Schlotterbeck
F. Hoffmann-La Roche Ltd
Grenzacherstrasse 124, Basel
CH-4070 Switzerland
goetz.schlotterbeck@roche.com
Automation and Miniaturization in NMR
47
Co-Author(s)
Alfred Ross,
Hans Senn
Currently NMR measurements are performed in tubes of 5mm diameter and a detection volume of about
500µL. Miniaturizing the NMR measurement has many advantages the most important are: (i) the intrinsic higher
sensitivity of the miniaturized detection coil leads to a decrease of the experiment time and thus potentially to a
higher sample throughput of mass-limited samples and (ii) the use of costly deuterated solvents can significantly
be reduced, and concomitantly the spectral artifacts from solvent impurities. NMR measurements using a new
1mm TXI Microprobe (Bruker) with an active sample volume of 2.5 µL are reported. This is the first microliter
NMR probe with optimized coil geometry for use with individual capillaries of outer diameter of 1 mm. The probe
offers significant advantages over previous and other analytical-chemical NMR technologies: an increased mass
sensitivity by a factor of 4 compared to the conventional setup and spectra with very low-solvent background. We
demonstrate the potential of the probe for structure elucidation of mass- and volume-limited samples and microbore
HPLC-NMR coupling on selected examples from pharmaceutical research. In addition applications with high
sample throughput (HT-NMR) for quality control of large sample arrays are shown. This also includes the automatic
sample preparation of 1mm capillaries.
8:30 am Wednesday, February 4 HT Chemistry – Analytical Room B3
Russell Scammell
Argenta Discovery Ltd
8/9 Spire Green Centre
Flex Meadow
Harlow, Essex CM19 5TR United Kingdom
russell.scammell@argentadiscovery.com
Automation and Mass Spectrometry: A Love – Hate Relationship?
Today’s mass spectrometer interface systems operate on principles that have remained fundamentally unchanged
for over 10 years although the method of automated sample introduction has probably experienced the most
significant changes over this time period. This presentation will initially provide a brief history of the interfaces and
sample introduction techniques that have emerged over the past decade. The discussion will move into areas
that are now key to the successful operation of an analytics laboratory supporting both the needs of Discovery
Chemistry and Bioananlysis. The paradigm shift to non MS-centric systems embracing the automation, integration
and miniaturisation (AIM) concept has greatly impacted on sample introduction. The factors of ever increasing
time pressures and sample numbers in today’s industry will be shown to have been the single driving force in the
areas of automated sample preparation/purification/analysis, HPLC column technologies, auto-sampler/fraction
collection technologies and interface hardware. The presentation will conclude with a look to the future, including
the area of chip based technologies and how the emergence of multiplexed interfaces are having an impact on
future autosampler designs.
PODIUM ABSTRACTS