Rapid Identification of Explosives and Other · 2017. 12. 6. · Need for speed •Applications...

Rapid Identification of Explosives and Other Substances of Forensic Interest

Presented by: Dr. Richard SleemanScientific Director, Mass Spec Analytical Ltd

Who we are

• A spin-out of of British Aerospace, established over 20 years in Bristol

• We design and build in the UK mass spectrometer ion sources and field transportable mass spectrometers

• We are ISO 17025 (UKAS) accredited and provide forensic services to law enforcement organisations and private corporations around the globe

• Our expert evidence involving trace detection has been presented to courts of law for thousands of cases

©2017 Mass Spec Analytical Ltd.

Alternatives to GC and LC

• GC and LC-MS are well established techniques over many years

• Main objective was to separate-out the target substance for analysis

• i.e. only one substance goes into the mass spec at a time – which in turns help eliminate matrix effects

• Needed retention time and mass spec spectrum


Need for speed

• Applications that require rapid identification and high selectivity (identification point criteria) need a new approach

• Nowadays, mass spectrometers can do a lot more

• For many compounds you no longer need to separate out the different constituents

• That being the case, chromatography is no longer a requirement – especially for small molecule applications such as drugs and explosives.


Conventional methods

• GC and LC – Time, chemicals, gas, glassware

• Conventional trace substance detection methods are time consuming and expensive

• Location of traces lost

• Evidence may be compromised during testing process

Collect•Shake item

over covered surface

Dissolve

•Debris dissolved in solvent & filtered to remove particulates

Prepare sample

•Resultant liquid reduced using nitrogen blow-down

Analyse GC/MS or LC/MS


Intro to Thermal Desorption

• We have developed a range of thermal extraction ion sources (TEIS) for testing particles, liquids and vapour

• We couple the TEIS devices to Sciex triple quad and QTOF mass spectrometers controlled by our bespoke application software

• Fast, no sample preparation, ideal for field deployment and suitable for a wide range of substances.

• The result is a product that can detect illicit drugs, explosives, and many other substances with virtually no false positives

• The system can test hundreds of samples per hour with no loss of performance

TEIS-3200-HB Hot Block Desorber with Sciex API3200 Triple Quad Mass Spectrometer ©2017 Mass Spec Analytical Ltd. 6

The simpler the process, the less that can go wrong….

LCMSWith LCMS, you have to show that every item which may come into contact with an exhibit is clean:

• Gloves

• Tweezers

• Swab (if used)

• Solvent used to extract the trace

• Vials and caps

• Syringes

• Derivatising agents

• etc., etc.

Thermal DesorptionWith TEIS, you take a swab and analyse it directly, all you have to prove is that the swab (and by inference, the hands holding it) are free of contamination:

• Swab (if used)

• Hand/glove holding it

The TEIS is self-purging so there is no clean-up required between tests

© 2017 Mass Spec Analytical

Peer-reviewed study validates method

A recently published paper* demonstrates the capability of using thermal tandem mass spectrometry (MS/MS) for the identification of substances of abuse and related compounds without the need for chromatography.

• MS/MS was shown to be capable of the identification of the same drugs within the samples as the conventional method of GC/MS, but with better sensitivity and shorter analysis times.

• The run times of chromatographic techniques can vary from a few minutes to hours per sample. For the analysis of drug samples by GC/MS, a 15-min run time is typical.

• Quasi real-time vs. 9s for autosampler

*The paper, published in Rapid Communications in Mass Spectrometry, 15 April 2016 is authored by CM Fletcher, Department of Physical Sciences, University of Kent at Canterbury, and R Sleeman, Mass Spec Analytical Ltd.


How reliable is MS/MS without chromatographic Separation? MS/MS spectra of a sample suspected of containing LSD at collision energies of 20 eV (top left) and 30 eV (bottom left) compared with a NIST MS/MS library spectrum of LSD at 22 eV (top right) and 32 eV (bottom right).

TIC of -MRM (6 pairs): from Sample 2 (Wet paper samples appx 20 ng) of Explosives on Paper swabs.wiff (Heated Nebulizer) Max. 5.1e5 cps.

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.941 81 121 161 201 241 281 321 361 401 441 481 521 561 601 641 681 720 760

Time, min

0.0

2.0e5

4.0e55.1e5

In

..

.

0.61 1.471.28

0.85 1.08

XIC of -MRM (6 pairs): 350.983/61.988 Da from Sample 2 (Wet paper samples appx 20 ng) of Explosives on Paper swabs.wiff (Heated Nebulizer... Max. 2.0e4 cps.

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.941 81 121 161 201 241 281 321 361 401 441 481 521 561 601 641 681 720 760

Time, min

0.0

1.0e4

2.0e4

In

..

.

0.85

1.08 1.47

XIC of -MRM (6 pairs): 261.971/61.988 Da from Sample 2 (Wet paper samples appx 20 ng) of Explosives on Paper swabs.wiff (Heated Nebulizer... Max. 1.6e4 cps.

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.941 81 121 161 201 241 281 321 361 401 441 481 521 561 601 641 681 720 760

Time, min

0.0

1.0e4

1.6e4

In

..

.

1.061.24

0.41

XIC of -MRM (6 pairs): 226.010/196.000 Da from Sample 2 (Wet paper samples appx 20 ng) of Explosives on Paper swabs.wiff (Heated Nebulize... Max. 4.5e4 cps.

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.941 81 121 161 201 241 281 321 361 401 441 481 521 561 601 641 681 720 760

Time, min

0.0

2.0e5

4.0e5

In

..

.

0.60 1.28 1.47

Examination of explosives from swabs


Swab 1 Swab 3Swab 2 Swab 4 Swab 5 Swab 7Swab 6 Swab 8

PETN

NG

TNT

TIC of +MRM (10 pairs): from Sample 4 (13478F04) of 13478F.wiff (Heated Nebulizer) Max. 1.2e7 cps.

1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4600 700 800 899 999 1099 1199 1299 1399 1498 1598 1698 1798 1898 1997 2097 2197 2297 2397 2496 2596 2696

Time, min

0.00

5.00e6

1.00e7

In

..

.

3.19

4.745.244.23

3.742.681.64 2.15

XIC of +MRM (10 pairs): 304.155/105.034 Da from Sample 4 (13478F04) of 13478F.wiff (Heated Nebulizer) Max. 6.9e6 cps.

1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4600 700 800 899 999 1099 1199 1299 1399 1498 1598 1698 1798 1898 1997 2097 2197 2297 2397 2496 2596 2696

Time, min

0.0

5.0e6

6.9e6

In

..

.

3.19

4.744.232.68 3.74 5.241.66 2.15


1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4600 700 800 899 999 1099 1199 1299 1399 1498 1598 1698 1798 1898 1997 2097 2197 2297 2397 2496 2596 2696

Time, min

1000

1500

1840

In

..

.


1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4600 700 800 899 999 1099 1199 1299 1399 1498 1598 1698 1798 1898 1997 2097 2197 2297 2397 2496 2596 2696

Time, min

0.0

1.0e6

1.7e6

In

..

.

4.74 5.24

1.643.20 3.74 4.222.15

Examination of drugs from swabs


Swab 1 Swab 3Swab 2 Swab 4 Swab 5 Swab 7Swab 6 Swab 8

Heroin

THC

Cocaine

Quantification with deuterated standards


TIC of +MRM (10 pairs): from Sample 92 (Her : D9 Stds2 08/04/15) of 12126A Plastic Note Project.wiff (Ion Spray) Max. 3.4e6 cps.

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0Time, min

0.0

1.0e6

2.0e6

3.0e6

3.4e6

In

te

n.

..

0.57

4.272.544.723.881.52 9.482.99 7.165.68 9.045.16 7.64 9.963.41 8.558.11 11.3910.8910.442.06

XIC of +MRM (10 pairs): 370.165/328.155 Da from Sample 92 (Her : D9 Stds2 08/04/15) of 12126A Plastic Note Project.wiff (Ion Spray) Max. 4.3e5 cps.

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0Time, min

0.0

2.0e5

4.0e5

6.0e5

In

te

n.

..

4.274.72

2.992.54 3.883.411.520.575.685.16

2.069.489.04 9.967.64 11.3910.8910.448.557.16 8.11

XIC of +MRM (10 pairs): 379.165/335.100 Da from Sample 92 (Her : D9 Stds2 08/04/15) of 12126A Plastic Note Project.wiff (Ion Spray) Max. 2.8e5 cps.

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0Time, min

0.0

1.0e5

2.0e5

3.0e5

4.0e5

4.5e5

In

te

n.

..

7.169.48

7.64 9.048.55 9.96

11.3910.448.11

5.684.272.54 3.41 3.881.52 4.72 5.162.06 2.99

Analysis of explosives using SWATH



BMSS* Inter-laboratory Comparison

＊British Mass Spectrometry Society, Ambient Ionisation Special Interest Group Inter-laboratory Study, 1 June 2016

• BMSS set out to test five different ambient ion source techniques with 5 different types of mass spec• Mass Spec Analytical (lab AIG17 in the report) is one of three labs to successfully detect all the target

substances in the trial. The other two successful labs used an Atmospheric Solids Analysis Probe method.

High Security events: case study

• High sensitivity and selectivity of the TEIS-Sciex MS system render it ideal for screening large venues, concert halls or stadia

• High sensitivity delivers a better chance of identifying a threat

• High selectivity reduces the chances of false alarms

• Mobile systems, mounted in vans, are in use by the UK police to screen high-security events


Scentinel deployed as a mobile trace detection system

Choose your mass spec

API3200 V-Series

X500R QTOF• Ideal for Unknown Substance Screening

• Available Q2 2018, based on the Sciex X500R QTOF Mass Spectrometer

• First High-Resolution portable QTOF mass spec for accurate mass measurements in the field. Massively increases the substances that can be detected.

• Delivers real-time and retrospective analysis in a single package

• Ideal for targeted detection

• Available now, based on the Sciex API 3200 Triple-Quad and other V-Series Mass Spectrometers

• Combines high-sensitivity and selectivity with a rugged, reliable compact package

• Deployed with North American Border Agencies


Further reading and References

C. M. Fletcher, R. Sleeman. Rapid Identification of Seized Controlled Substances and Related Compounds by Tandem Mass Spectrometry without Chromatography. Rapid Commun. Mass Spectrom. 2016, 908.

A. Wilson, C. Aitken, R. Sleeman, J. F. Carter. The Evaluation of Evidence for Auto Correlated Data in Relation to Traces of Cocaine on Banknotes. Appl. Stat. 2015, 64 Part 2, 275.

A. Wilson, C. Aitken, R. Sleeman, J. F. Carter. The Evaluation of Evidence Relating to Traces of Cocaine on Banknotes. Forensic Sci. Int. 2014, 236, 67.

K. A. Ebejer, R. G. Brereton, J. F. Carter, S. L. Ollerton, R. Sleeman. Rapid Comparison of Diacetylmorphine on Banknotes by Tandem Mass Spectrometry. Rapid Commun. Mass Spectrometry 2005, 19, 2137.

R. Sleeman, J. F. Carter, Forensic Science - Explosives, in Encyclopedia of Analytical Science, (Eds: P. Worsfold, A. Townshend, C. Poole). Elsevier, 2005, pp. 400–406.

R. Sleeman, S. L. Richards, I. F. A. Burton, J. G. Luke, W. R. Stott, W. R. Davidson, Detection of Explosives Residues on Aircraft Boarding Passes, in Vapour and Trace Detection of Explosives for Anti-Terrorism Purposes, (Ed: M. Krausa). Springer, PO Box 17, 3300 AA Dordrecht, Netherlands, 2004, pp 133-142.

M. Tam, P. Pilon, H. Zaknoun. Quantified Explosives Transfer on Surfaces for the Evaluation of Trace Detection Equipment. J. Forensic Sci. 2013, 58, 1336.


Thank you!www.msaltd.co.uk


Rapid Identification of Explosives and Other · 2017. 12. 6. · Need for speed •Applications...

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