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?

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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?

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IconNMR configuration

How to use SmartDriveNMR? Operation Modes

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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

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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

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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

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SmartDriveNMR report – recommended follow-up

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Settings Results

OPTime, 2 min 1D 1H Sample in wet DMSO

SmartDriveNMR report – recommended follow-up

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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

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100%

NUS%

49%

STOP

1D 1H

24%

256

Time Efficient 13C NMR Parameter Optimization for Number of Scans

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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

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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

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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

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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

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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

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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

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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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