Analytical chemistry education activities at University of ...€¦ · measurement uncertainty in...

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Analyticalchemistry

education activities at University of

TartuIvo Leito

[email protected]

EcoBalt 2018Vilnius

Contents

• Validation of LC-MS methods– State of the art– Tutorial papers– The online course

• Estimation of Measurementuncertainty in chemical analysis

• Usage modes of the online materials• International master programmes• Eurachem 2018 Workshop

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www.akki.ee

All links and slides

LC-MS as technique

• Liquid chromatography mass spectrometry• The most powerful technique for determination of

low levels of organics in difficult matrices• LC-MS: many adjustable parameters

– In LC– In MS

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Checking that the methodperforms as required is not trivial!

Validation is BIG in LC-MS!

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ValidationGuidelines?

Validation guidelines

• Generally very useful, but ...

– Often inconsistent terminology• e.g. accuracy vs trueness, ...

– Often very general• Choosing concentrations? How many replicates? Spiking

levels? How many days? ...– Sometimes conflicting recommendations– Usually LC-MS is not addressed

• Except e.g. 2002/657/EC

26.10.2018 6sisu.ut.ee/lcms_method_validation/

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Our aims were:1. Give a critical overview of the state of the art of

LC-MS method validation– Including comparisons of the relevant guidance

materials

2. Draw attention to the LC-MS specific aspects– e.g., ionization suppression by matrix effects

3. Give recommendations on problematic issues in validation of LC-MS methods


Outcome:Two-part tutorialreview inAnal. Chim. Acta

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- Tutorial review on validation of liquid chromatography–mass spectrometrymethods: Part I. A. Kruve, R. Rebane, K. Kipper, M.-L. Oldekop, H. Evard, K. Herodes, P. Ravio, I. Leito. Anal. Chim. Acta 2015, 870, 29-44. http://dx.doi.org/10.1016/j.aca.2015.02.017

- Tutorial review on validation of liquid chromatography–mass spectrometrymethods: Part II. A. Kruve, R. Rebane, K. Kipper, M.-L. Oldekop, H. Evard, K. Herodes, P. Ravio, I. Leito. Anal. Chim. Acta 2015, 870, 8-28. http://dx.doi.org/10.1016/j.aca.2015.02.016

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Features

• Specific LC-MS issues– Ionization, matrix effects, MSn selectivity, ...

• Main validation guidelines are reviewed and compared– With every performance parameter

• Recommendations are given how to determineperformance parameters– Synthesis from guidelines and our experience

• General workflow of LC-MS method validation ispresented


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Tutorial review on estimating LoDon the exampleof LC-MS

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- Tutorial on Estimating Limit of Detection on the example of LC-MS analysis: Part I. H. Evard, A. Kruve, I. Leito. Anal. Chim. Acta 2016, 942, 23-39. http://dx.doi.org/10.1016/j.aca.2016.08.043

- Tutorial on Estimating Limit of Detection on the example of LC-MS analysis: Part II. H. Evard, A. Kruve, I. Leito. Anal. Chim. Acta 2016, 942, 40-49. http://dx.doi.org/10.1016/j.aca.2016.08.042

Hanno Evard

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On-line course: LC-MS Method Validation

sisu.ut.ee/lcms_method_validation/

Online LC-MS Validation course• Validation: General• Performance parameters

– Selectivity, Identity• Incl specifics of LC/MS

– Linearity, linear range, sensitivity– Precision, Trueness, Accuracy

• Including matrix effects– Stability– LoD, LoQ, CCα, CCβ

• Including specifics of LC/MS– Ruggedness, Robustness

• Glossary• Literature


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Course contents• Theoretical basis as well as practical skills• Detailed and example-based treatment• More than 50 short video lectures by 6 teachers

– Excel videos demonstrating calculations• Numerous tests and calculation exercises

– Understanding of main concepts– Calculation exercises from real life situations– Feedback is given

• On-line software (some functionality)26.10.2018 15

Videos ...

• Using slides:

... or ...

• Pen and whiteboard:


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Discussion dialogues

• Two proffessionals discuss a problematicsituations: one asks for help and the other onegives suggestions


Labvideos


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Excel videos explainingcalculations

• Initial calculation files can be downloaded


Worked examples

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Self-tests


Online validation software

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MOOC: Autumn 2017 edition424 registered participants from 71 countries

2326.10.2018

Overall completion rate: 37%Completion rate of those who started: 67%

Interested?• Without registration: the materials are freely

available 24/7:

• Registered participation:– Forums– Graded tests– Free of charge (digital certificate)

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LC/MS Validation MOOC – third edition:Nov 27, 2018 – Feb 08, 2019

Registration is open at:sisu.ut.ee/lcms_method_validation/

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sisu.ut.ee/measurement

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On-line course: Estimation of measurement uncertainty in chemical analysis

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Our goal• Web-based teaching material for

– Independent learning to estimate measurement uncertainty in real-life situations

– On-line reference point of explanations of concepts and approaches

– Support for auditorial teaching of metrology inchemistry at UT, summer schools, etc

– Offering as MOOC

• Required previous knowledge– General analytical chemistry knowledge

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Course contents

• Theoretical basis as well as practical skills• Detailed and example-based treatment

– Modeling (ISO GUM)– Within-lab validation (Nordtest)

• Close to 50 short video lectures– Supplemented by textual explanations and downloadable

slides and calculation files• Numerous tests and calculation exercises

– Understanding of main concepts– Calculation exercises from real life situations– Feedback is given

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sisu.ut.ee/measurement

Uncertainty course completionrates up to now

Year Registeredparticipants

Successfully completedOverall Who started

2014 270 52% 67%2015 489 34% 60%2016 757 40% 67%2017 363 41% 68%2018 521 42% 61%

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• The uncertainty course will again be offered inspring 2018

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„Usage modes“

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LC/MS MethodValidation


On-line course forindependent

learningavailable any time

anywhere

On-line referencepoint

of terminology, explanations and

self-testingpossibilities

Running asMOOC

with registeredparticipation, on-linecounseling, gradedtests and certificate

Course materialfor running trainingcourses e.g. by labs

Support touniversity teaching

Students can bedirected here e.g. for

self-testing

MOOCs vs „traditional“ teaching

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Aspect Conventional university course

Practitioner training (short) course MOOC

Interaction between students and teachers Direct Direct Remote

Possibility to deliver the course simultaneously to many participants Low Low High

Level of self-discipline needed from participants Average Average High

Time constraints, time to “digest” the knowledge Not a problem Serious time

constraintsNot a

problem Possibility of independent homework Possible Usually impossible Possible Possibility of hands-on problem-solving Possible Possible (within the

time constraints) Possible

Possibility of teamwork Possible Possible (within the time constraints) Not easy

Possibility of experimental work Easy Possible, but not easy Not possible

Possibility of working with participants of uneven level or preparation Difficult but doable Difficult Possible

Possibilities of meaningful assessment of obtained knowledge Wide possibilities Difficult Possible

Danger of cheating during knowledge assessment Can be made low Can be made low Can be

high Costs of setting up the coursea Medium Medium Medium Costs of running the coursea High High Low Travel and accommodation costs Can be high Can be high None

I. Leito, I. Helm, L. JalukseAnal Bioanal Chem, 2015,407,1277–1281

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Applied Measurement ScienceMaster’s Programmeams.ut.ee

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AMS Outline• Interdisciplinary 3+2 master's degree programme• Cross-sectorial

– Physical measurements– Chemical measurements (chemical analyses)– Metrology– Quality systems– Economic and legal

aspects of measurements• Tuition in english

The education thatstudents will get is

of very broadapplicability

www.ut.ee/ams

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Programme structureObligatory Module (45 ECTS)

Courses: Measuring and Instrumentation, Measurement Data Processing, Lab of Physical Measurements, Practical Chemical Analysis Methods, Lab of Chemical Analysis Methods, Fundamentals of Metrology, Metrology in Chemistry, Seminar in Measurement Science,

Quality management

Elective Module (30 ECTS, courses can be chosen from the list)Courses: Atomic Spectroscopy, Materials Characterization and Testing, Measurements in Biochemistry, Measurements and the Law, Economic Aspects of Measurements, Signal

Processing, Chemometrics, Environment and Measurement, Electrochemical Measurement and Analysis Methods, Nanometrology, Quality Systems etc

Optional Subjects(6 ECTS, any courses can be chosen university-wide)

Practical speciality training(9 ECTS, internship placement in industry or analysis or calibration laboratories)

Master’s thesis(30 ECTS, reasearch project with a topic related to measurement science)

www.ut.ee/ams26.10.2018

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Measurement Science inChemistry

• Internationalconsortium

• 9 countries– Estonia, Slovenia,

Bulgaria, France,Portugal, Poland,Finland, BelgiumIreland

• 11 universities• 9 Summer schools during 2008-2016

www.msc-euromaster.eu

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Excellence inAnalytical ChemistryErasmus Mundus

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Excellence in Analytical Chemistry• Four European universities excelling in

different fields:

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Fundamentals of analytical chemistry,metrology in chemistry, quality assurance,

socio-economic aspects

Organic and bioorganic analysis, advanced separation methods, mass

spectrometry

Industrial analysis, process control and monitoring

Advanced analytical devices, sensors, miniaturization,

electrochemistry

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Excellence in Analytical Chemistry

• Full-fledged contemporary analytical masterdegree programme (120 ECTS)

• Tuned to the job market needs– Metrology topics– Socio-economic aspects– Practical placement

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EACH Programme structure:

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University of TartuFundamentals of analytical chemistry,

metrology in chemistry, quality assurance,socio-economic aspects

Uppsala UniversityOrganic and

bioorganic analysis, advanced separation

methods, mass spectrometry

University of Lyon

Industrial analysis, process control and monitoring

Åbo AkademiAdvanced analytical

devices, sensors, miniaturization,

electrochemistry

Year 1: Fundamentals + Placement 60 ECTS

Year 2: Specialisation + Master’s thesis 60 ECTS

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Validation of targeted and non-targeted methods of analysis

• Examples of issues addressed:– Validation of targeted methods: where are we?– Validation of non-targeted methods – differences from

targeted methods– Detection of a multitude of (unknown) components in

complex samples, criteria for identification– Managing the huge amounts of complex data from non-

targeted methods– Software solutions for validation

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Many thanks to the team!Course

development:Lauri Jalukse Irja Helm Hanno Evard

Anneli Koit Maarja-Liisa Riin Karin AnuKruve Herodes Oldekop Rebane Kipper Teearu

Video, web design, admin:

Enno Kaasik Triin Marandi Lehti Pilt Esta Pilt Toomas PetersellJuho Jalviste26.10.2018 43

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Thank you for your attention!

Slides and links:www.akki.ee

Questions, requests:[email protected]

LC/MS Validation MOOC – third edition:Nov 27, 2018 – Feb 08, 2019

Registration is open at:sisu.ut.ee/lcms_method_validation/

Analytical chemistry education activities at University of ...€¦ · measurement uncertainty in...

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