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Meeting Training Needs for Mass Spectroscopists

Achieving Reliable Mass Spectrometry Data: Back to BasicsAAMG - RSC

6 June 2006

Dr Andrew J ReasonM-Scan

M-Scan

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The M-Scan Group of CompaniesMass Spectrometry Consultants and Analysts

• Founded 1979 in Iver (UK), moved to Ascot in 1983

• Four laboratories: Wokingham, UK (M-Scan Ltd)Geneva, SwitzerlandFreiburg, GermanyWest Chester, PA, USA

• Offices in Germany (Bonn, Munich), North England, and representation in South Korea and India M-Scan

© M-Scan 2006

The M-Scan Group of CompaniesMass Spectrometry Consultants and Analysts

• 25 years of experience in the provision of analytical services by mass spectrometry.

• GLP & cGMP certification, FDA inspected.

• 100% confidentiality.

• Agreed turnaround time of projects.

• 40 highly qualified MS scientists.

• Peer review of all reports.

• 20 state of the art mass spectrometers together with ancillary equipment (HPLC, GC, TLC, TOC, IR …).

M-Scan

© M-Scan 2006

The M-Scan Group of CompaniesMass Spectrometry Consultants and Analysts

M-SCAN EXPERTISE

Solution of analytical problems in the following areas using an appropriate and cost-effective combination of MS and chromatographic techniques:

• OFEC:

• Biopolymers / Pharmaceuticals

• Essential Oils• Contaminated Foods• Environmental monitoring• Oils and Fats• Forensic Analysis • Fire Investigations

• Synthetic Polymers• Detergents • Petrochemicals• Additives• Odour analysis• Fuels/Lubricants

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

M-Scan has been running training courses for Mass Spectroscopists for more than 20 years. The initial courses were aimed at training Mass Spectroscopists to use the new technique of FAB-MS originally pioneered by M-Scan in the early 1980’s.

Meeting Training Needs for Mass Spectroscopists

Andrew Reason - M-Scan Ltd, Wokingham

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M-Scan

© M-Scan 2006

Meeting Training Needs for Mass SpectroscopistsM-Scan has made a commitment:

• to identify the training needs of the MS community within the areas of expertise serviced by M-Scan

• to develop courses to meet these needs.

Courses developed cater for the rapid growth and interest in mass spectrometry for investigation of a wide range of problems in:

• chemistry • biochemistry • pharmacology• forensic science• environmental analysis.

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

In recent years short courses have been offered utilising M-Scan’s mass spectrometry and chromatography expertise.

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

1. An Introduction to Mass Spectrometry

2. LC/GC - Mass Spectrometry

3. Choosing a Mass Spectrometer: the Right Tool for the Job

4. MS/MS Analysis and Interpretation: the Key to Structure Elucidation M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

5. Mass Spectrometry in Proteomics and Post-Translational Analysis

6. Advanced Biopolymer Mass Spectrometry: Protein, Carbohydrate & Oligonucleotide Sequencing

7. Product Characterisation of Biopharmaceuticals: Bringing a Protein to Market

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

8. Applications of Mass Spectrometry in Environmental Analysis

9. The Use of Mass Spectrometry in Forensic Analysis

10. Detailed Analysis of Petroleum Hydrocarbons in the Environment

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

Enquiries from:

• Company and Government Scientists - mainly lab based

• Company Senior Staff – mainly management roles

• Company Quality Control Staff

• Company Sales / Marketing Staff

• Academic Institutions - Staff and Students

Meeting Training Needs for Mass Spectroscopists

Andrew Reason - M-Scan Ltd, Wokingham

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M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

Participants on M-Scan Training Courses

Co/Gov ScientistCo Senior StaffCo QC staffSales / MarketingAcademic StaffAcademic Student M-Scan

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Meeting Training Needs for Mass Spectroscopists

Ancillary Issues:

• Cost of course and discounts

• Cost of accommodation and travel

• Location and possibility of course at client’s site

• Duration

M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

Important factors:

• Expertise of course presenters.

• Backgrounds of the course participants.

• Lectures lasting 50 to 60 mins maximum.

• Lectures interspersed with problems and tutorials to cement understanding.

• Practical demonstrations to illustrate MS best practices and to produce data for use in problem classes and tutorials.

• Course Manuals / Notes.

• Each course limited to about 10 participants to ensure good interaction.

• Certificate of attendance.M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

Provides: • An introduction to the basic technology• Consideration of the different types of instrument• Interpretation of spectra• Lectures• Discussion Sessions• Problem Tutorials• Practical Demonstrations.

An Introduction to Mass Spectrometry(M-Scan Course MS01)

M-Scan

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Meeting Training Needs for Mass Spectroscopists

The Introductory Course covers:

The most important Ionisation techniques used in Mass Spectrometry, including:

Electron ImpactMatrix Assisted Laser DesorptionElectrospray

Descriptions of the most common mass analysers, and how to choose the correct combination for the problem under study. M-Scan

© M-Scan 2006

Meeting Training Needs for Mass Spectroscopists

Emphasis is placed on:

• Interpretation of Mass Spectra

• Problem Classes with examples from the research literature and the Lecturers’ experiences

• Practical Demonstration of some of the sample handling and Mass Spectrometric techniques. The mass spectrometers used in the practical session include a Q-TOF (quadrupole orthogonal acceleration time of flight) instrument.

Meeting Training Needs for Mass Spectroscopists

Andrew Reason - M-Scan Ltd, Wokingham

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M-Scan

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Meeting Training Needs for Mass SpectroscopistsThe Course is designed for scientists who have:

• little or no experience of mass spectrometry • wish to take advantage of the technology for their

investigations, either using in-house facilities or the services of a contract laboratory such as M-Scan.

The Course aims to:

• enable the participants to begin studies involving mass spectrometry

• provide a sound basis for subsequent in-depth training, perhaps in the more specialised courses offered by M-Scan.

© M-Scan 2006

M-Scan

The Mass SpectrometerConsists of three basic components

Electron Impact (EI)Chemical Ionisation (CI)Fast Atom Bombardment (FAB)Field Desorption (FD)Electrospray Ionisation (ES)Atmospheric Pressure CI (APCI)Matrix Assisted LaserDesorption Ionisation (MALDI)

Magnetic sectorQuadrupoleTime-of-flightIon trap

Electron MultiplierPhotomultiplierMultichannel plateArray

ION SOURCE MASS ANALYSER DETECTOR

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M-Scan

ES/FAB/MALDI fragmentationEXAMPLE 1 : Small molecules e.g. pharmaceuticals

Protonation will be on a heteroatom, and fragmentation may be driven from this site or it may be charge - remote

C10H7NO4

© M-Scan 2006

M-Scan

ES/FAB/MALDI fragmentationINTERPRETATION :

• DBEs = 8 looks very aromatic – 2 rings ?

• m/z 188 is a simple water loss – alcohol or acid

• m/z 178 looks like a –CO or C2H4 loss from the quasimolecular ion

• C2H4 loss is very unlikely since it would leave only 3 Hydrogens for the remaining 8 Carbon atoms! Furthermore m/z178 may be a water addition to a very reactive ion at m/z 160

• m/z 160 looks like a –CO loss from m/z 188 and taken together these ions strongly suggest the presence of a carboxyl group

• Note how there is a virtual absence of fragmentation below m/z160 again indicating a very stable bicyclic aromatic core

© M-Scan 2006

M-Scan

INTERPRETATION :

• We can now draw some trial structures and using these design further experiments, for example, derivatisation of possible functional groups followed by MS “mass shift” analysis in order to refine the structure of the unknown

• In this way, Example 1, which is the Malaria gametocyte activating factor from mosquitos, was identified as the following structure:

Reference : Nature 392, 289-292 (1998)

ES/FAB/MALDI fragmentation

N

OH

COOH

OH

M-Scan

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Meeting Training Needs for Mass Spectroscopists

After attendance on this course participants should be able to:

• Choose the best MS technique to solve a particular problem.

• Interpret mass spectra including Electron Impact and MS/MS data.

• Adopt the best practice for experiment design.

• Understand the contribution of MS to structure elucidation.

Meeting Training Needs for Mass Spectroscopists

Andrew Reason - M-Scan Ltd, Wokingham

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M-Scan

© M-Scan 2006

Meeting Training Needs for Mass SpectroscopistsSummary of Main Considerations

• Cost, location, duration.

• Expertise of course presenters.

• Course content.

• Effective teaching methods in particular with the use of problems and tutorials to cement the understanding.

• Providing relevant examples and case studies for a number of applications.

• Constant revision of courses to keep them up to date.

Meeting Training Needs for Mass Spectroscopists

Andrew Reason - M-Scan Ltd, Wokingham