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