Reaction Monitoring: InsightMR
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1 Reaction Monitoring: InsightMR Robert Krull Senior Applications Scientist Pittsburgh April 2016 Innovation with Integrity
2 Outline Introduction InsightMR Flow Tube InsightMR Software Setup Data Analysis with Dynamics Center
3 Reaction Monitoring What is it and Why are we Doing it? Reaction completion determination In-situ yield determination Reaction understanding: mechanistic information Extracting kinetic parameters Stability, degradation studies Dissolution Bio transformations Process control - PAT FDA providing guidelines for PAT
4 Techniques for Reaction Monitoring Calorimetry LC-UV MS, GC, GC-MS IR In-line (in-situ) measurements possible! NMR» At-line» In-line» On-line Quantitative by default: no need to calculate response factors! Information rich: possible to elucidate the structure of starting materials, products, and intermediates.
5 * Patent Pending What is InsightMR? Hardware Software InsightMR flow tube* InsightMR software package
6 InsightMR Flow Tube April 14, 2016
7 Concept InsightMR flow tube is an insert for virtually any Bruker 5 mm NMR probe. Enables online monitoring of chemical reactions in real-time under real conditions Fast and continuous transfer of reactions mixtures from a reaction vessel into the flow tube and back Continuously circulates the liquid from a reaction vessel through the NMR probe. The changing composition of the liquid in the vessel, i.e. the progress of the reaction, can be continuously monitored. Temperature control from the vessel to the probe and back achieved by running sample lines through temperature controlled heat transfer fluid
8 Basic Schematic InsightMR Package Customer Supplied NMR Magnet
9 Flow Tube Assembly Overview
10 Easy to Replace Flowcell Tube is easy to remove Cell protector doubles as an installation tool
11 Laboratory Setup Coventry, UK
12 Enabling parallel acquisition of data from different spectroscopies
13 Flow Behavior Delay of Transfer (a) Integral corresponds to 15 mm composition min Composition in pump was changed to 100% (c) After min change visible in NMR (d) After min 90% of target composition reached (e) After ~ min ~100% target composition reached (b) (e) (d) <1-2 min is possible by adjusting the flow rate to 2-3ml/min Adjustment of hardware (length diameter) also possible. (4 m length, 1 ml/min flow, 0.5 mm i.d. capillaries) (a) (c) Pump contributes ~100 ul to delay of concentration step propagation.
14 Line Shape Test 10 mm sucrose Stopped flow, 16% Flow 1 ml/min, 17% Flow 1 ml/min, after re-shimming, 15%
15 Fun Facts Available in 2 lengths: 4m and 7m Cell is 5mm tube Volume ~600ul Filling height ~40mm Sample Capillary Material: PTFE i.d.: 0.5mm Capillary volume (in & out): 4m ~1.6ml, 7m ~2.7ml Temperature Range: -5C to 60C Maximum Pressure (sample): 10bar Maximum Flow Rate (sample): 5ml/min.
16 InsightMR Software Integrates acquisition and analysis Gives the ability to assess and adjust acquisition parameters in real time April 14, 2016
17 Integration of Acquisition and Analysis Click Click Acquisition Spectra Display
18 Getting Started with InsightMR Obtain and install a copy of the InsightMR software* Available on the Topspin 3.5 DVD. Version 3.5pl5 recommended. Can be downloaded at Registration required Search for insightmr Most up-to-date version Necessary components Can install in parallel Import configuration Prosol Cortab User specific files etc. *Windows available now Linux version in beta testing
19 Getting Started with InsightMR Obtain a Reaction Monitoring license NOTE: Valid Topspin 3.x license also required
20 InsightMR Software and License License request form at
21 InsightMR Software and License Using search term insightmr produces hits for software download and license request as top 2 hits.
22 InsightMR Demo License NOTE: Not instantaneous, typically 1-2 business days
23 License File No REACTION_MONITORING_1 Feature
24 Getting Started with InsightMR After software has been installed and licensed Open Topspin CF expinstall Optional: Acquire a spectrum Close Topspin Open InsightMR Set default automation mode Verify license OK Check solvents and parameter sets
25 Getting Started with InsightMR Method Center active Solvents and Parameter sets OK
26 Getting Started with InsightMR After software has been installed and licensed Open Topspin CF expinstall Optional: Acquire a spectrum Close Topspin Open InsightMR Set default automation mode Verify license OK Check solvents and parameter sets Let s get started!
27 Getting Started with InsightMR LIVE DEMO
28 Getting Started with InsightMR Utilizes ICONNMR EZ-setup interface Choose sample position Choose or enter experiment name Choose solvent
29 Getting Started with InsightMR Utilizes ICONNMR EZ-setup interface Choose experiment parameters Optional: Add information to title
30 Getting Started with InsightMR Utilizes ICONNMR EZ-setup interface Adjust acquisition parameters Set number experiments (data points) Time between experiments (data points) Set reaction t=0 Adds experiments to the queue
31 Getting Started with InsightMR Experiments have been added to the queue
32 Getting Started with InsightMR Click on Start Choose mode Click on Start to initiate the run
33 Experiment Delay Change Delay between points modified during run
34 Modifying Acquisition Settings Find the IconNMR/InsightMR window (may be in background) Click on the Configuration button
35 IconNMR Configuration Settings holder InsightMR uses User ReactionMonitoring
36 Experiments Straightforward set up K_PROTON (zg30) K_WATER (zgcppr) K_NOESY1D (ns=8, NO presat) K_WET & K_WETDC (no deuteration, no lock) User selects number of peaks to suppress Program does the rest: Shim on 1 H, optimized for variety of solvents Scout scan to find solvent peaks Calculate shaped pulse for suppression Run suppressed spectrum Automatic referencing
37 IconNMR Configuration Settings Parameter sets available in InsightMR Easy to add your own parameter sets
38 Adding Experiments and Parameters
39 Solvents When importing a configuration it may be necessary to Restore default solvents if the new H solvents are not visible Don t forget to enable Show no locking solvents
40 Adding New Solvents Step 1 - Topspin rename. E.g. test & add description
41 Adding New Solvents Step 2 - IconNMR 4
42 Lock and Shim
43 Adding New Solvents Step 2 - IconNMR 4 5
44 Protonated solvents Shimming: lctshim Special treatment for unlocked acquisition Set solvent dependent search range for Shim signal Activate RGA and compensation for flowing liquid (convcomp) Selective 1H shimming All automatically done with commandline parameter flow xau lctshim flow
45 Diels Alder Chemistry, NON-Deuterated Solvent CH3CN 25C DMF Maleic Anh. Product acetonitrile
46 Diels Alder Chemistry, NON-Deuterated Solvent
47 IconNMR Configuration Settings InsightMR uses Easy Setup Mode Separate IconNMR configuration files may be needed if normally running in the standard mode
48 IconNMR Configuration Settings Separate IconNMR configuration files can easily be saved and recalled for different automation modes.
49 Key Benefits A single interface for automated acquisition control, and interactive processing and analysis On-the-fly acquisition changes as needed based on real-time kinetic data Straightforward experiment set up. Default experimental parameters provided for both deuterated and non-deuterated solvents Rapid and effortless handling of hundreds of stacked spectra Supports acquisition, processing and analysis of series of 1Ds (different nuclei), interleaved experiments and multiple samples in parallel
50 InsightMR Team Project Manager Anna Codina Software Peter Neidig Mark Garvey Flow Tube/Hardware Martin Hofmann Ulrich Braumann Applications/Development Peter Gierth Eberhard Schweizer Nicola Tonge Aitor Moreno Rob Krull
51 Copyright Bruker Corporation. All rights reserved.
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