RIGHT S O L U T I O N S | RIGHT PARTNER
Automation of Full-Scan GC-MS analysis using IXCR
11/06/14 – John Quick
ALS Environmental
ALS Global Footprint
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Argentina
Chile
Ecuador
Peru
Bolivia
Brazil
Columbia
Mexico
USA
Canada
Burkina FasoGhana
Mali
Saudi ArabiaTurkey
Romania
Poland
FinlandRussia
China
Laos
Namibia
South Africa
Tanzania
Malaysia
Thailand
Taiwan
Australia
New Zealand
New Caledonia
Fiji
Hong Kong
Singapore
Indonesia
Portugal
Czech Republic
NorwaySweden
Mongolia
Germany Denmark
United KingdomIreland
Kazakhstan
KyrgyzstanSpain
Italy
Netherlands
Zambia
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ALS in the UK and Ireland
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ALS in UK and Ireland:
• 14 laboratories/offices
• 880 staff
• Annual revenue in excess of £58 million
• Corporate office in Aberdeen
} ALS Life
Sciences
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The ALS Philosophy
• Our business leaders are all operational people who
understand how to run efficient, customer-centred
laboratories.
• We believe that innovation is a source of competitive
advantage. We focus those efforts where we think we can
improve the service we offer our clients.
• Innovation is shared with colleagues on a global basis.
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ALS Environmental U.K
• Severn Trent Laboratories (STL) purchased by ALS in
2013
• 3 Laboratory Sites
– Coventry
• Wastewater / Contaminated Land
– Wakefield
• Potable Water
– Chester
• River Dee intake protection
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Wakefield - Full Scan GC-MS
• Wakefield Laboratory
– Routine
• Use of HPLC, GC-MS, GC-MSMS and LC-MSMS for a range
of target compounds including Pesticides, Phenols, PAH
– Non-routine
• Package of analysis includes GC-MS full-scan for target
list of compounds and tentative identification of non-
target compounds by library searching
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Wakefield - Full Scan GC-MS - Overview
• Traditional Sample prep
– 1L sample
– DCM extraction
– Evaporation to 1ml
– Analysis by GC-MSD in full-scan mode
• Data Processing
– Quant analysis of target list of compounds
– Non-target compounds by PBM search of NIST/WILEY
libraries
– Manual construction of combined report
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Wakefield - Full Scan GC-MS - Issues
• No deconvolution of data
– Closely eluting peaks – not “pure” mass spectra leading to
problems with identification.
– Peaks that are “under” the baseline missed
• Manual time consuming process
– Review “hits”
– Compare with blank
– Produce report
• Experienced / skilled analysts required
– Consistency of judgement
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Coventry – SVOC Analysis
• Semi-volatile Organic Compounds (SVOC) based on EPA
8270 suite of compounds
• Dirty water samples
• Extraction by LLE/SPE
• Analysis by GC-MS in SIM/Scan mode
• Target list of about 80 compounds quantified from SIM
trace
• Tentatively Identified Compounds (TIC) report from Scan
trace. Semi-quantitative against nearest internal
standard.
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Coventry – SVOC Analysis
• TIC Reports – Current
– Generate TIC report from Chemstation
– Edit TIC report
• Manually compare with blank by overlaying
chromatograms – remove compounds in blank
• Check peak assignments – difficult in dirty samples
• Check for un-integrated peaks – manually integrate,
library search and add to report
– Takes experienced analyst 1 day to do 20 samples
– Without deconvolution peaks will still be missed!
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SVOC Chromatograms
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Deconvolution - Objectives
• Enhanced service to clients
– More peaks more reliably identified
– Lower reporting limits
• Improve productivity
– Bring automation to manual process
– Release experienced analysts to other tasks
• Basic Requirements
– Reliable deconvolution of GC-MS datafiles and automated library searching
– Semi-quantification against nearest internal standard
– Comparison against blank sample
– Capability for batch processing
– Export results to Excel for post-processing
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GC-MS Full Scan Process
• ACD IXCR software successfully introduced into our Wakefield
lab beginning of 2013. Starting process of implementation into
Coventry lab for SVOC/TIC
• GC-MS full scan process
– Analysis on GC-MSD – quantification of target compounds using
Chemstation
– Deconvolution of blank control sample on ACD software
– Batch deconvolution of sample datafiles using “Compare to control”
– Data review
– Export results to Excel
– Generation of sample report using in-house macros
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IXCR Options
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IXCR Options
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IXCR Options
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IXCR Options
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IXCR Options
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IXCR Options
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IXCR Options
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Data Review
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Data Export
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Excel Output
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Excel post-processing
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Excel post-processing
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Report generation
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Sample Report
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Sample Report
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Summary of Benefits
• Enhanced service to customers
– More peaks, more reliably identified at lower reporting
levels
• Productivity / Efficiency
– Automation of manual process
• Time / cost savings
• Reproducibility
– Release of experienced analysts to other tasks
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Next Steps
• Implement in Coventry laboratory for SVOC
• IntelliTarget for target compounds?
• Acquire NIST in ACD labs format to increase speed and
accuracy
• Use of spectral databases to characterize sample points
• Potential for use with high resolution LC-MS scans??
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Thank you!
• Any Questions?
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