© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann...
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Transcript of © Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann...
© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
LC-(SPE)-(Cryo)NMR(/MS) as Routine Analysis Technique:Instrumentation and Software
Dr. Ulrich BraumannBruker Biospin, Rheinstetten
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Agenda
• Startup SampleTrack
• Startup Preparation Program PrepGilsonST
• Startup NMR Program TopSpin and ICONNMR
• Setup Orders
© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Startup instruments and prepare the System
Dr. Ulrich BraumannBruker Biospin, Rheinstetten
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare SampleTrack PC
• Login to the SampleTrack PC, typically with
- User: samtrack
- passwd: bsts
• Check that the following programsare running
- SampleTrack Webservice
- SampleTrack Communicator
- SampleTrack Client
• If not, start the programs
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare SampleTrack PC
• In the SampleTrack Client check go to the page instrument status
• Typically all instruments will show“not responding” as the programs onthe other computers are not started
• Follow the instructions on the nextpages to startup the instrumentprograms and in parallel observe inthis window that the connectionsare established.
• The instrument programs whichcommunicate with SampleTrack are
- Compass Sample Track communication
- ICONNMR
- PrepGilsonST
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare SampleTrack PC
• Clean up Sample orders
- Attention: During the next steps the automation programs are started.
- If they detected the barcode of samples which have open orders in SampleTrack, the preparation or NMR/MS measurement may start immediately.
• Therefore it is recommended to search for open orders from previousruns and –if required-delete them.
- Go to the pageSample Orders
- Search forNot yet finished Samples
- Check if this orders shallbe really executed. If notdelete them.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare PrepGilsonST
• Start PrepGilsonST, and select the“Profiler” application.
- Gilson remain disconnected– This is normal!
- A white bar must indicate aof SampleTrack and PrepGilsonST
- In SampleTrack Client must change from “not responding”to “preparation loop not started”
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Start PrepGilsonST
• Do Preparation/Start preparation Automation
- The program must connect to the liquid handler.
- The LiquidHandler must start reading barcodes.
- In the SampleTrack Client the status must turn to green
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare ICONNMR & SampleJet
• On the TouchScreen of the SampleJet check if the correct mode is selected
- Do not use “manual mode” – switch to the correct shuttle diameter.
- Ensure that you have selected the correct diameter.
- Remove any sample from the magnet and ensure that the shuttle with the correct diameter is in the magnet.
• Open the ICONMR- Configuration
- Load the configuration for the SampleJet automation
- Check settings for locking, shimming, ATMA.
- If shimfile-loading is activated, check that the define shimfile is up-to-date.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Start ICONNMR
• Start ICONNMR automation, do not define any experiments
• Start the automation procedure
- Select “SampleTrack(SampleJet).
- In SampleTrack the status must turngreen “online waiting for orders”.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare HyStar & MS Control
• Identify the standard method path ofHyStar (“D:\data” or “D:\methods”).
• From this path open the SampleTable“openaccess.xml” – or create it.
• The SampleTable should have one lineand the method should be thesame as used during the analysis.
• Enter the acquisition window ofHyStar with this line.
- The Acquisition window must openand HyStar must show green status.
- The MS control software must correctlyopen and show green status.
- If you cannot open HyStar/MS control withthe method selected for the measurements,STC will not be able either!
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Prepare HyStar & MS Control
• Start the program SampleTrack Communication.
- Start in online mode = yes
• HyStar will vanish in the background.
• The program must start and show status ready for all parts.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Finish
• All instruments are now ready to run experiments.
• If the any experiment start immediately
- you have samples in the Liquid handler, NMR sample changer or LC-MS changer which still have open order in SampleTrack.
- Go to page Prepare SampleTrack PC and check if the listed orders are still wanted. Either delete the orders or remove the rack with the corresponding samples from the instruments.
© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Process Samples
Dr. Ulrich BraumannBruker Biospin, Rheinstetten
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Setup Orders - manual
• Have the barcoded rack/wellplate with the samples ready.
• In SampleTrack do File/New
- Enter the ID of the tay (upper text like “RCK000183”)
- Enter the geometry identification of the tray.
- Select the sample position in the tray from the displayed layout.
• Select the “supermethod” that defines the complete process from the preparation to the measurment in the NMR and LC/MS
- If required customize the supermethod, for example to disable certain NMR experiments or disable the NMR or MS measurement part completely.
- Note: Disabeling the prepartion is not possible, as this also includes the assigment of the ID of the original sample to the position of the SampleJet tube/LC-MS well.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Sample Preparation
• Open the door of the hood
- Place the tray with the samples into the liquid handler.
- Ensure that an unused rack with SampleJet tubes and a unused wellplate for MS aliquot is available.
(Note: If a number of samples already were prepared from the source rack, the original destination rack(s) must be available. I.e. you may have to return them from the SampleJet or LC-MS autosampler)
• Close the door of the hood
- The liquid handler must start scanning the barcodes to identify the new samples.
- The liquid handler will look for available destination racks.
- The preparation will start automatically.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
Sample Preparation
• The destination for a sample preparation will be automatically determined by sample track.
• Samples will be prepared symmetrically from source to destination.Sample #1A1, #2A2, #13 B1 etc (i.e. not submitted sample position will remain empty in the destination).
• The destination rack will remain reserved for the source rack.
• As consequence.
- You can remove a not completely filled destination rack from the liquid handler to start the NMR or LC-MS measurements.
- The preparation will continue into another free rack (if a suitable rack is found).
- However the empty spaces in both destinations racks are not available for other source racks!
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
NMR Measurement
• Remove samples from the liquid hanlder
- Open the door of the hood.
- Remove the a rack with the SampleJet tubes.
- Close the door of the hood.
Note: If the preparation of one rack is not completely finished, the preparation will pause until the original SampleJet rack is back in the liquid handler!
• Insert the tray into the SampleJet
- Ensure that current shuttle diameter matches the samples tube diameter.
- At the SampleJet touchscreen select “Load rack”.
- Select the position and place the rack into the caroussel.
- Confirm with done.
- The SampleJet starts automatically to read the barcode of the rack
- ICONNMR will start executing the NMR experiments for the found samples.
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© Bruker BioSpin 2008; File: braumann_jena_080828.ppt; Version: 2008-08-28; By: Dr. Ulrich Braumann
LC-MS Measurement
• Remove samples from the liquid hanlder
- Open the door of the hood.
- Remove the a rack with the SampleJet tubes.
- Close the door of the hood.
Note: If the preparation of one rack is not completely finished, the preparation will pause until the original SampleJet rack is back in the liquid handler!
• Insert the tray into the LC-MS autosampler
• Submit the ## name of the wellplate.
- The orders for this wellplates will be take from SampleTrack and will start automatically.
- It is recommended to run 1-3 blank runs before the first real sample, to equilibrate the LC-MS system.