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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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