the smart spectrometer - bruker€¦ · case study: 3 / 4 april 14, 2016 11 expert: “spectrum...
TRANSCRIPT
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Björn Heitmann, Ph.D.
Applications Development
Pittsburgh – April 2016
The Smart Spectrometer
Innovation with Integrity
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CMC-assist-
Summary NMR choices
When to run which experiment?
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Researcher e.g. SmartDriveNMRRequests HSQC
Higher confidence
result
Structure Verification = SmartDriveNMR!
User approaches instrument with question, sample description and restraints
• Instrument decides which experiments to run with which parameters• Automatic data analysis • Yields result with confidence level ( - )• Decides if- and which other experiments are required to achieve user desired confidence level • If user allotted time permits, system sets up runs follow up experiments
Auto-result
withconfidence
level
OK
Automatic decision Auto-result II
OK
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SmartDriveNMR: supported experiments
• More scans (better SiNo)• Analyzes data and determines if and how many scans are needed for improvement• If time permits, sets up and runs the experiment
• Suppression • Determines whether e.g. water suppression in DMSO-d6 would make sense and
determines required ns based on 1D1H
• HSQC• Determines if an HSQC would add more information and thus confidence • Based on the 1D1H determines required ns for HSQC
• HMBC • Determines how much more confidence would be gained by an HMBC • Based on the 1D1H determines required ns
• 13C• Determines if a 1D13C would add more information / confidence • Based on the 1D1H determines ns for 13C (not probe dependent yet)
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SmartDriveNMR:Confidence on Structure verification
April 14, 2016 5
Definition of Confidence (C)
C = f ((ST, SQ)i, Complexity)
• ST: Spectrum type, e.g. 1H• SQ: Spectrum quality• Complexity of assignment problem
evaluated based on structure and n measured spectra (i=1 to n)
- Amount equi. atoms- Prediction quality- Spectrum overlap- Diversity in signals and atoms
• Desired Confidence is set as Stars in the GUI
• Confidence ranges between 0 to 5 Stars
• Confidence is calculated for the current verification project
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Instrument decides which experiments to run
6April 14, 2016
There are three needed green lights to measure the next experiment:
1. Is another measurement useful?
2. Is enough time left?
3. Is the desired confidence not reached yet?
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SmartDriveNMR: Setup in IconNMR
April 14, 2016 7
• Question at hand: structure verification
• Default SmartDriveNMR parameters are set in IconNMR
• One box to tick to activate SmartDriveNMR
• Set the default desired confidence the default maximum instrument time per sample
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CMC-assist-
Summary SmartDriveNMR Results
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Case Study: 1 / 4
9April 14, 2016
Expert: “Small and simple molecule with a nice and disperse spectrum – assignment straight forward” No follow-up experiment
SmartDriveNMR:1D 1H Consistent, Confidence 3.5 Stars No follow-up experiment
Final: Consistent, Confidence: 3.5 Stars
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Case Study: 2 / 4
10April 14, 2016
Expert: “Small and simple molecule with an ok spectrum – assignment possible” maybe more Scans?
SmartDriveNMR:1D 1H Consistent, Confidence 2.8 Stars More Scans
Final: Consistent, Confidence: 3.2 Stars
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Case Study: 3 / 4
11April 14, 2016
Expert: “Spectrum dominated by Water (and Solvent DMSO)” Suppression
SmartDriveNMR:1D 1H Consistent, Confidence 0.3 Stars Suppression
Final: Consistent, Confidence: 3.1 Stars
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Case Study: 4 / 4
Expert: “Structure is complex and 1H spectrum is not easy to assign” HSQC
SmartDriveNMR: 1D 1H Consistent, Confidence 2.1 Stars HSQC
Final: Consistent, Confidence: 3.9 Stars
Expert: “Even though structure looks complex and worth an HSQC, the 1H spectrum is fairly easy to assign” No HSQC
SmartDriveNMR:1D 1H Consistent, Confidence 3.5 Stars No HSQC
Final: Consistent, Confidence: 3.5 Stars
M = 422 g mol-1
M = 520 g mol-1
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SmartDriveNMR: HSQC statistics
When are HSQCs suggested:
• In 32% of > 1000 1D test cases (Ø 300 – 500 g/mol)
• More likely for high MW compounds
0%
20%
40%
60%
80%
100%
Ratio of suggested HSQCs on top of 1Dby MW
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Summary
14April 14, 2016
• SmartDrive NMR carries out experiments automatically in an optimized way based on the previous experiment
• Optimization of spectrometer’s time while keeping best quality in results - saving user time “in front of the spectrometer”, e.g. day, night, week ends
• Both NMR experts and non expert benefit
• Interactive / Manual Structure Verification using CMC-assist 2.4
• SmartDriveNMR is new and available in TopSpin 3.5 fully integrated in Iconnmr - just a few clicks to try it !
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Thank you!
Acknowledgements:
• Many NMR users, customers and colleagues for input, ideas and critics
• Come, see us for a demo
• … and we really appreciate your feedback!
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Innovation with Integrity
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