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Transcript of 1 NMR For The Serious Organic Chemist Easy Open Access, High Sensitivity, High Throughput NMR...
![Page 1: 1 NMR For The Serious Organic Chemist Easy Open Access, High Sensitivity, High Throughput NMR Platform Easy Robust Fast Efficient Economical Controllable.](https://reader034.fdocuments.net/reader034/viewer/2022050714/56649e365503460f94b24e6f/html5/thumbnails/1.jpg)
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NMR For The Serious Organic ChemistEasy Open Access, High Sensitivity, High Throughput NMR Platform
• Easy• Robust• Fast• Efficient• Economical• Controllable• Flexible
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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Answers Needed From NMR
Copyright © 2008 by Protasis Corporation, All Rights Reserved
90%
9% 1%
Did I makethe stuff?What is thisstuff?Other
Source: Survey of 40+ Industry and Academia by Protasis Corporation
Bonus: yield (ERETIC)Percentage Of Samples
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IntroducingThe One-Minute NMR System
• Optimized Liquid Handling• Application-Tuned CapNMR Probe• Exclusive Spectrometer Interfaces• Robust Software• Collaboration With Partners and End-
Users
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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What is it?
Everyone wants a magic wand!
Leap/CTC PALLiquid Handler
CapNMR ProbeNMR Spectrometer
ACD/Automation Server
E-Mail OrWeb Site
You Just Log In Samples
One-Minute NMRManages The Details
ACD/Web Librarian
Did I make it?
Yield?
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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MRM CapNMRTM Microcoil Probes
• 5-10 microliter flow cell = 8 – 15 microliter samples
• Best mass sensitivity• Short acquisition times• Concentration > 1mM works well
UseCapNM
R
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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One-Minute NMR Software
• Secure Log-In• Individual sample
entry and Molecule upload
• Automated Quality Control and Performance Monitoring
• .ZIP/.CSV Sample lists and molecule upload
• Bar-code support• Open SQL Server• Custom Fields• LDAP Login
Web-Based Open Access Sample Queue Management
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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Click…
Minutes Later…In your InBox
Hot-linked E-mail reportIntegrated ACD/Web Librarian
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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The Advantages of CapNMR (micro-scale)
Use MS vial directly or 50-100µg with a filter vial
Add solvent, centrifuge
Click Run To Start
Before you get back to the lab, e-mail arrives.
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The Advantages of CapNMR (micro-scale)
Scaled-Down Purifications
Scrape off a spot into filter. Add DMSO-d6, spin.
Collect fractions at analytical scale HPLC
Exchange to minimal DMSO-d6
A
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The Advantages of CapNMR (micro-scale)
A
Can you spare a few µg? No waiting at the NMR Lab! No return trip!
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The Advantages ofCapNMR (quantitation)
• NMR is the most accurate form of quantitation (with no standard)
• Accurate quantitation is important for screening
• Tube NMR has problems, tuning and shimming affects signal strength and quantitation
• CapNMR is the ideal ERETIC and quantitation platform
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Automated Quality Controland Performance Monitoring
Automation Requires Continuity
• QC Samples– Check S/N, line shape, extra
signals– Run at regular intervals or on
demand– Certified sealed vials available
• Pressure monitoring and History• Gas manifold and bottle
integrity checks
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ACD/Labs Structure Confirmation and DatabasingAdaptive Experiments Get Results, Save Time
1D Proton
>= 1D Proton Acceptance Level
HSQC
ConfirmedRejected
>= AVG(HSQC + 1H1D) Acceptance Level
YESNO
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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LEAP PAL
• Fast• Low Volume Pickup• Low Dead Volume• Syringe-Only
Technology• Flexible Sample
Storage • Dilute /
Reconstitute• Sample Return
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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The advantages of going tubeless…
•No shimming between samples
•No washing tubes
•Minimal sample transfer
•Efficient storage
•Disposable
•Economical
Incredible Time Savings
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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Effortless Solvent Management
• Vacuum Degasser– Smooth
MicroFlows
• Helium Sparging / Blanketing– Protect
Expensive Deuterated Solvents
• Automatic System Checks
Helium
NE
ED
LE
V3
SAMPLES
SY
RIN
GE
The Deuterated Solvent Conditioning Module mounts conveniently in the door of the Discovery Tower
Vacuum
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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SO
LV
. A W
AS
TEINJECT
V2
LOOP
SAMPLES
NE
ED
LE
SY
RIN
GE
High Pressure PUMP
Copyright © 2008 by Protasis Corporation, All Rights Reserved
Ca
pN
MR
PR
OB
E
High Throughput Sample Loading
Sample Return Option
1-2 min.
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Robust Operation
• Multiple maintenance counters• Automatic instrument reboot• E-mail alerts• Inline filtration with pressure
monitoring• Improved NMR Error Reporting• 2+ years of continuous
operation
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• Varian– Sun TCP/IP
Sockets
• Bruker– Windows Drive
Mapping– SGI / Linux TCP/IP
Sockets
• OthersEasy instrument
integration
Spectrometer Interfaces
Copyright © 2008 by Protasis Corporation, All Rights Reserved
Router
RSH(a.shimFile)RPAR(a.experiment, "all")
SETCURDATAXCMD("gpro")
RGASTOREPAR("NS", a.scans)
STOREPAR("SW", a.sweepWidth)STOREPAR("o1p",
a.centerOfSpectrum)exptime = CalcExpTime();
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Actual Use Case: Major Pharmaceutical Company
A
Before One-Minute NMR
• 3 NMR Systems• 5mm Tubes• Open-Access• Chemists Prepare Samples• Chemists Interpret Spectra• Actual use: 600 samples / month.• Capacity: 1900 samples / month
“If utilization gets to 100% there is a hanging.”
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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Use Case: Major Pharmaceutical Company
2 One-Minute NMR Discovery Tower Systems + ACD/Labs AutomatedStructure Confirmation
• Actual Use: 4000 / month• Capacity: 8000+ / month • Structure Verification for Every Sample• 1D Verification, 60% Accurate• Water Suppression• ERETIC Quantitation
“Different dynamics now: Verification, used to be done by chemists. It is easy with familiar compounds, but hard when chemistry changes. The demand went way up from Parallel Medicinal Chemistry. It puts NMR back in the game for structure verification.”
A
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Actual Use Case: Major Pharmaceutical Company
Before * After
Direct Labor and Utilization
Labor FTEsActual Use
“I just scan the barcode label and click Start.”
A
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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One-Minute NMR™Open Access, High Throughput NMR Platform
• Secure Open-Access Web Interface• Integrated LEAP/CTC Liquid Handler
– Multiple vial/plate sample formats• Safe Solvent Management
– Degassing, Sparging, Blanketing– Solvent Selection
• High-Throughput Sample Loading and Analysis
– 1-minute loading, 1-scan 1D proton• Closed-Loop Spectrometer Control
– Run -> Idle ->Run– Error handling
• Automated Structure Confirmation– Integrated 1D+2D ACD/Labs– Automated/adaptive experimental design– DataChord Integration
• E-Mail reporting– HTML Plate Maps– Error Alerts– Forgotten Passwords
Exclusive Attributes Productivity Features• QC Samples• Priority Samples• Night Samples• Probe Clean• Solvent Select• Sample Return• Sample List Importing• Structure Confirmation• Custom Counters• Custom Fields -> NMR Dataset
Parameters• SQL Database• Pressure Monitoring• Solvent System Checks• Macros• Dilution• User List Importing• Automatic instrument reboot
Copyright © 2008 by Protasis Corporation, All Rights Reserved
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Help spread the word!
www.protasis.com508-481-4163
Now NMR is easier and faster
One-Minute NMR