Innovation with Integrity
Easy NMR II The Intelligent Spectrometer Dr. Christoph Freudenberger Applications Development – Head of Validation Bruker Users’ Meeting Hilton Head Island, SC – March 2019
Easy NMR: New Software towards the Intelligent Spectrometer
2 March 12, 2019
Advanced Processing
Smart Automation
Spectrometer Adjustment New software for calibration of spectrometer: AutoCalibrate & AssureSST
Easy NMR: New Software towards the Intelligent Spectrometer
3 March 12, 2019
New software for data acquisition: SmartDriveNMR & CMC-q
Advanced Processing
Smart Automation
Spectrometer Adjustment
4 March 12, 2019
SmartDriveNMR Advanced acquisition tool for synthesis control in open access
Running a NMR facility, you might be familiar with…
5 March 12, 2019
Do this with solvent suppression?
What is the appropriate
NUS-amount for an HSQC?
?
What does SmartDriveNMR do?
6 March 12, 2019
SmartDriveNMR requests further experiment
• Additional data will only be acquired if it is useful for answering your question.
• SmartDriveNMR reports it’s reasoning • Good quality spectra • Automatic analysis
consistency & concentration structure
HSQC because…
analysis optional
How to use SmartDriveNMR?
7 March 12, 2019
IconNMR configuration
How to use SmartDriveNMR? Operation Modes
8 March 12, 2019
Operation Mode Behaviour
FIXperiment Experiments are carried out exactly as they are set up by the user WITHOUT parameter optimization. The measurement time results directly from the set up experiments. You get what you ordered
OPTime Only the experiments highly beneficial for the given synthesis control task that fit in the given time are carried out with optimized parameters. You get time-optimal spectrometer usage
MAXperiment All experiments that are technically possible and fit into the given time, will be carried out with optimized parameters. You get the maximum possible number of experiments
Settings Results (time needed depends on sample concentration)
OPTime, 60 min 1D 1H in < 3 min
MAXperiment, 60 min 1D 1H, HSQC, 1D 13C, HMBC in ca. 50 min
Settings Results (time needed depends on sample concentration)
OPTime, 120 min 1D 1H, HSQC, 1D 13C, HMBC in ca. 100 min
MAXperiment, 120 min 1D 1H, HSQC, 1D 13C, HMBC in ca. 100 min
How to use SmartDriveNMR? Operation Modes
9 March 12, 2019
Reasoning mechanism for additional measurements
• > 25 rules to decide on further experiments
• For xample: Number of CH2-groups; chemical shift predictions in comparison to CH-groups
12 March 12, 2019
Why measure an
HSQC? 1.8-2.5 ppm
2.3-2.8 ppm
Output to user: “STRUCTURE-COMPLEXITY; CH2- and CH-groups should be distinguishable.”
SmartDriveNMR reports
13 March 12, 2019
SmartDriveNMR report – recommended follow-up
14 March 12, 2019
Settings Results
OPTime, 2 min 1D 1H Sample in wet DMSO
SmartDriveNMR report – recommended follow-up
15 March 12, 2019
Settings Results
OPTime, 2 min 1D 1H
15%
NUS in a fail-safe way
• How to determine the appropriate sampling amount (NUS%)? • From the available input, estimate conservatively NUS%
• At acquisition time, start with a lower NUS% • Increase NUS% stepwise • Until high data quality is reached stop
16 March 12, 2019
100%
NUS%
49%
STOP
1D 1H
24%
256
Time Efficient 13C NMR Parameter Optimization for Number of Scans
17 March 12, 2019
1024 • From 1D 1H number of scans (NS) is estimated
conservatively for 1D 13C
• At acquisition time S/N is determined at low NS • NS increased stepwise and S/N is measured • Until desired S/N is reached stop
NS
STOP 600
1D 1H
18 March 12, 2019
CMC-q High-throughput tool for large sample libraries
Innovation with Integrity
CMC-q – Your Tool for Quality Control
What is CMC-q? • A tool for the acquisition and analysis of many samples in one batch
What is the typical customer for CMC-q? • Quality control of samples in the context of CROs
• Check compounds before fragment-based screening
• Compound library control
• Anybody that needs to measure many samples in a pre-defined manner
Innovation with Integrity
Fully Integrated Workflow
Set-Up Acquisition Analysis View & Edit Reporting
• Set-Up: Simple dialogue to submit your experiments in one go
• Acquisition: Handled full-automatically, simply put your samples in your sample changer
• Analysis: Full-interpretation of data including, assignment, multiplets, integrals, concentration, purity, and water-content
• View & Edit: Change interpretations as needed
• Reporting: Export your results to excel or csv
Innovation with Integrity
New Setup Dialog
Is it complicated to setup experiments in CMC-q?
• Only few things to select to start your experiments
• Workflow based on structure-data (sd) files
• Streamlined acquisition schemes for your verification task
• With the new dialogue it´s even easier
Innovation with Integrity
Create your own Verification
Is it possible to use my own parameter sets?
• Yes!
• You can create your own acquisition schemes (=verifications)
• Simply select the desired parameter sets
• Mix predefined and customized parameter sets
• You can also select from our predefined acquisition schemes
Innovation with Integrity
View, Edit, Report…
• The CMC-assist is the viewer for the results of CMC-q – it comes for free with buying CMC-q
• Export your results to excel by a simple click
• Easy overview to your data in the plate view
• Sort and navigate to your sample in the table view
• Highlight samples outside your concentration corridor
plate view table view
Would like to know more?
• Webinar recording available! • See us for demos and quotes! • Become an early adopter! • Available with TS 4.0.6/ 3.6.1
27 March 12, 2019
Easy NMR: New Software towards the Intelligent Spectrometer
28 March 12, 2019
New procedure for phase and baseline correction: apbk Advanced Processing
Smart Automation
Spectrometer Adjustment
29 March 12, 2019
apbk Reliable automatic phase and baseline correction
Probably, you know spectra like…
Physical limits like high Q-factors in the resonator circuits or background signals from solids lead to not so perfect spectra
30 March 12, 2019
19F 13C
13C apbk
apbk Automatically Perfect Phase and Baseline
• New command in TopSpin and CMC-assist: apbk • Designed especially for the use with “problematic” X nuclei spectra (13C, 19F, 31P) • Performs better in automation than apk; abs
31 March 12, 2019
13C apk; absn
19F apbk
apbk Automatically Perfect Phase and Baseline
• New command in TopSpin and CMC-assist: apbk • Designed especially for the use with problematic X nuclei spectra (13C, 19F, 31P) • Performs better in automation than apk/apks/apkm combined with abs/absd/absn
32 March 12, 2019
19F apk; absn
apbk – What are the Options?
Available Options • -po phase only • -bo baseline only • -n do not write integration regions
Intended Use
• X-nuclei: 13C, 19F, 31P Force for other nuclei
• -f force usage on other nuclei • Please let us know if and how it works!
Availability
• Topspin 4.0.6/3.6.1
33 March 12, 2019
Easy NMR: New software available in TopSpin 4.0.6/3.6.1
34 March 12, 2019
apbk for 13C, 19F, 31P
SmartDriveNMR & CMC-q
AutoCalibrate & AssureSST
Advanced Processing
Smart Automation
Spectrometer Adjustment
See us for demos & quotes! Early adopters welcome!
35 March 12, 2019
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