MicroFlow NMR
description
Transcript of MicroFlow NMR
MicroFlow NMR
Advances in NMR Automation for
2006
Why MicroFlow? Sensitivity
EconomySimplicity
• Make less, use less, dispose of less BETTER ECONOMICS!• Miniaturized RF Design HIGHER MASS SENSITIVITY!• Easier to shim and install SIMPLICITY!• Utilizes modern sample formats => VERSITILITY!• Enhanced signal-to-solvent ratio INFORMATION QUALITY!• Excellent salt tolerance LESS SAMPLE-TO-SAMPLE VARIATIONS!• Excellent fluidics PRESERVE SAMPLE CONCENTRATION!• Uni-directional flow MAXIMIZE SPEED, MINIMIZE CARRY-OVER!• Fused silica/FEP pathways EXCELLENT SOLVENT COMPATIBILITY!• Diverse range of sample management options
MAXIMIZE YOUR MAGNET AND SPECTROMETER INVESTMENT!• Compatible with Varian, Bruker, JEOL, Waters, and other NMR and fluidic platforms
The Heart of MicroFlow NMR:The CapNMR Probe
Great Sensitivity, Easy Operation, Excellent Spectral Quality
Data Courtesy of Mike Frey, JEOL USA, Peabody, MA USA
CapNMR Performance
Get an independent assessment of performance from a major
NMR vendor who has used our probe - Download 30-page specifications document at
www.jeolusa.com/nmr/nmrprods/cap_probe.html
Product PositionsPrecious Sample Analysis Turnkey Solutions
NMR
Gronquist et al., JACS 2005, 127, 10810 Jansma et al., Anal. Chem. 2005, 77, 6509
Precious Sample Analysis PositionDirect Injection
Sample VialsSample is easily dispensed from syringe to probe
Easy,Effective,Efficient
SimplePlumbing
To learn more about Direction Injection Loading, see the Protasis/MRM Technical Bulletin G0020 in the Tech Support Knowledge Base at www.microNMR.com
Precious Sample AnalysisFirefly Steriods
Semi-purified mixturethree major components total mass ~200 g1H NMR spectrum 32 scans
Semi-purified mixturethree major components total mass ~200 g1H NMR spectrum 32 scans
dqf-COSY spectrum 8 scans 512 complex incrementstotal time 3 h 45 min
coupled non-gradient HMQC spectrum 16 scans, 512 complex incrementstotal time 7 h
non-gradient HMBC spectrum baseline-subtracted in F164 scans, 460 complex incrementstotal time 21 h 45 min
NOESY spectrum 16 scans, 256 complex incrementstotal time 4 h 18 min
dqf-COSY HMQC HMBC NOESY
Spectral analysis allowed for complete structural characterization of all three major components, compounds 1, 8, and 13.
M. Gronquist et al., JACS 2005, 127, pp. 10810-10811
Precious Sample AnalysisNatural Products Dereplication
HPLC250 µg
~ 5 µg/well
Courtesy John Blunt, U. Canterbury, and Kirk Gustafson, NCI(see March 2006 Gordon Conf. On Natural Products Presentations at www.microNMR.com)
Precious Sample Analysis Assisted Direct Injection
• Semi-automated• Calibrated Delivery Volume• “Push-Button” Operation• Pressure Sensing
To learn more about Assisted Direct Injection, see the Protasis/MRM HTSL Technical Notes in the Manuals section of the Tech Support Knowledge Base at www.microNMR.com
Precious Sample Analysis Assisted Direct Injection Micro-SPE of Metabolites
Courtesy Andreas Kaerner, Eli Lilly, ENC 2004
Turnkey Solutions
Modern sample input formatWeb-based GUI control Decision-making SW
IN OUT
Secure Data Server
•Standard sample formats•Sensitivity•Capacity•Integration/functionality•Automation•Decision-making•Multi-solvent/open access•Easy to Use
# of
Sam
ples
$/S
amp
le
Protasis One Minute NMR
Wash Station
Thermal Control
Injector option:return-to-vial or well
Port-in-ValveInjection!
Minimal sample dilution, minimal dead volume
Control/automation SW
One-Minute NMRTM
Turnkey Solutions for NMR
Liquid Handling1
NMR Instrument Control2
Solvent Management
Sample QueueAutomation
Open-AccessWeb Interface
ACD/Labs Processing and Databasing3
E-mail and Web Reporting
Productivity
1 Leap/CTC2 Varian or Bruker3 ACD/Labs
Sensitive CapNMRProbe
Protasis One Minute NMR Bruker DPX-400, 10µL Sample Volume in Well, 5µL Injection
A
B
C
Courtesy Bernhard GeierstangerGNF
1) Med. Chem. Support/ Library QC• 384-well plates
2) Walk-up Med. Chem. Analysis• Microvials
Protasis One Minute NMR Human Serum with High Throughput CapNMR
Urine
Serum
Carryover StudiesSingle rinse protocols, in
combination with injection port maintenance, reduce carryover to negligible values, well less than 1%
600MHz capillary NMR, ns,6410 g/10 L
Protasis Corporation
Protasis technology has been advanced though the support of:NIH RR14392, RR11755, HL56546, RR14661, RR16387, EB001626-01, RR15384, RR020239, NSF DMI-9523220
For More Information, Visit: www.protasis.com (product offering)
www.microNMR.com (technical support)
Sensitivity
EconomySimplicity
Graphics on this page complements of:• Mark O’Neil-Johnson, Sequoia Sciences• Wolfgang Peti, Brown University• Brad Bendiak, U. Colorado Health Sciences Center • Dave Detlefsen, Novatia• Jane Strouse, UCLA• Kirk Gustafson, NCI and John Blunt, U. Canterbury