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Fast Method Development using AutoSRM and autoSIM
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12.2610.648.13 8.42 9.756.365.375.214.69RT: 8.23SN: 506
Pentachlorobenzene Masstrace m/z
250 in fullscan acquisition
S/N 35
Pentachlorobenzene m/z 250 in SIM
acquisition S/N 506
Short refresher on SIM benefit
Pesticides in soils
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Fullscan TIC
Dichlorvos in SIM @ m/z185
Dichlorvos in SRM 185>109
Dichlobenil in SIM @ m/z171
Dichlobenil in SRM 171>136
Refresher on MS/MS benefit
Pesticides in herbs
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Method development using the classical set up with segments or windows
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Segment this…… 150 pesticides
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Method development using the classical set up with segments or windows
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N1T M_
• In SIM we need 3 ions/comp or 126 ions/segment • In MS/MS we need two transitions or 82 ions/segment • Manual set up leads to errors • Matrix injections leads to RT shift, compounds fall out of the
window, so often methods are made with compounds in two segments
• Many ions/ segment= lower dwell times= lower S/N
42 compounds in a segment
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Modern method development for single and triple quads
Fullscan
• Library search • List of compounds and RT
develop
• autoSIM or • autoSRM
GO
• Link to software • Acquire and quantify • Update method
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AutoSIM
GC and AS method
Chromatography OK?
no
Yes. Automation can start
FS run + lib search Compound list
Or… Start automation here
Click on the compound; A mass intensity list and S/N is shown; Click on the desired m/z Create a working list
Attach working list to Instrument method; Quantitation software
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Productivity Features: t-SIM
Acquisition - Timed
Link the working list; the work list is in fact now a database
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AutoSRM
1) Precursor ion selection
2) Product ion selection
3) Collision energy optimization
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AutoSRM
• Automates the following: • Creation of fullscan, product ion scan and SRM methods • Creation of sample sequences • Creation of data layouts for analyzing results • Selection of precursor, product and collision energies
End result showing optimized transition
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Timed-SRM Method Overview
Acquisition - Timed
Link the working list; the work list is in fact now a database
Pre and post times are adjustable; So in case of shift due to heavy matrix the compound is still inside the window
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GC-MS and MS/MS Method Development Workflow
Develop missing compound/ SRM or SIM
Add to database
Multi-component method
Automatic SIM or MRM method creation
Self -customized Auto-optimized
RT Update
My target compound
list Auto SIM Auto SRM
Just ask us for existing databases
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Analysis of 300 Pesticides – Segmented vs. Timed
Segmented SRM Timed SRM Closest compound to segment break: 5 seconds
Can lead to compounds disappearing in case of RT shift
Closest compound to segment break: 15 seconds
Average number of simultaneous transitions: 55
Average number of simultaneous transitions: 15 (4X higher dwell times- better sensitivity)
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AutoSRM User Case
• Created and optimized > 250 transitions for > 80 compounds
• Minimal user interaction over 24 hours
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TSQ 8000 Timed-SRM User Case result
Terbacil
Alachlor
Tolylfluanid
Pyridaben
Tea Analysis: 4 pg on-column
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TSQ 8000 Timed-SRM User Case result
Spiked ketchup Analysis: 50 ppb Example diazinon
12.5 13.0 13.5 14.0 14.5 15Time (min)
RT: 13.64AA: 1555401SN: 80040
RT: 13.63AA: 1047822SN: 6301
Top: Timed SRM: - S/N 80040 - response: 1555401 Bottom: Segmented SRM: - S/N 6301 - response: 1047822
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TraceFinder Method Sync
• Links TraceFinder Method with instrument method
• Enables: • Compound based acquisition setup
• Automated update of acquisition windows
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Method Sync – Automated RT Update
…updates both TraceFinder Method and Timed-SRM Method
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In Conclusion
Image courtesy of digital art FreeDigitalPhotos.net
• Auto SIM and auto SRM:
• Simplifies the method development • Speeds the method development up • Makes adding new compounds easy • Connects the instrument and quantifying method
• Timed SIM and SRM:
• Eliminates the need for cumbersome segmenting • Limits the number of ions per unit of time; • Thus ensuring optimal dwell time and increasing the signal
to noise
