Our on-line LC-MS Method Validation Course 2020-2021: Registration is open!

Validation_of_LC-MS_Methods_Online_CourseWe are glad to announce that the fifth edition of the online course LC-MS Method Validation created and organised by our Analytical Chemistry group is open for registration at the address https://sisu.ut.ee/lcms_method_validation/ !

The course will be offered as a Massive Open On-line Course (MOOC) during Nov 24, 2020 to Feb 05, 2021.

This is a practice-oriented on-line course on validation of analytical methods, specifically using liquid chromatography-mass spectrometry (LC-MS) as technique, mostly (but not limited to) using the electrospray (ESI) ion source. The course will also be of interest to chromatographists using other detector types. The course introduces the main concepts and mathematical apparatus of validation, covers the most important method performance parameters and ways of estimating them. The course is largely based on the two-part tutorial review:

The course materials assembled by the members of our group include video lectures, texts, tables, schemes, practical exercises, and numerous tests for self-testing. In spite of being introductory, the course intends to offer sufficient knowledge and mathematical skills for carrying out validation for most of the common LC-MS analyses in routine laboratory environment. The real-life analysis situations for which there are either examples or self-tests are for example determination of pesticides in fruits and vegetables, perfluoroalkyl acids in water, antibiotics in blood serum, glyphosate, and AMPA in surface water, etc. It is important to stress, that for successfully carrying out validation, practical experience – both in analytical chemistry as such and also specifically in validation – is crucial and this can be acquired only through hands-on laboratory work, not via an on-line course.

Participation in the course is free of charge. Receiving a digital certificate (in the case of successful completion) is also free of charge. Printed certificate (to be sent by post) is available for a fee of 60 EUR. Registration is possible until the start of the course. The course material is available from the above address all the time and can be used via the web by anyone who wishes to improve the knowledge and skills in analytical method validation (especially when using LC-ESI-MS).

Our LC-MS Method Validation e-course received quality label from HITSA!

Each year the Estonian Information Technology Foundation for Education (HITSA) recognizes the e-courses crested by Estonian educational institutions, that have demonstrated high quality in their online teaching. The main aim of this award is to improve the level of e-courses and to endorse those, that have shown excellence in their teaching.

The awarded quality label certifies the high level of the e-course and recognizes the authors for achieving excellent results in the implementation of e-learning to their teaching process. The importance of e-courses grows year by year. This was especially seen this spring when the majority of teaching and studying had to be done via the web because of the Covid-19 situation. 

This year our LC-MS Method Validation web course was honored to receive the quality label. Altogether 511 people from 77 countries registered to the course last autumn. The LC-MS Method Validation MOOC will start again in autumn 2020.

Congratulations on this well-deserved recognition to Ivo, Anneli, Riin, Maarja-Liisa, Hanno, Koit, Karin, Irja, and Asko from our analytical chemistry group!

EACH is featured in Analytical and Bioanalytical Chemistry!

The educational section of the leading analytical chemistry journal Analytical and Bioanalytical Chemistry, the ABCs of Education and Professional Development in Analytical Science has published a paper about the EACH programme: EACH (Excellence in Analytical Chemistry), an Erasmus Mundus Joint Programme: progress and success

The EACH programme is an Erasmus Mundus Joint Master Degree programme coordinated by our group. It has become one of the leading master’s degree programmes focusing on analytical chemistry within its short existence. The programme is run in cooperation by four top European universities: in addition to the coordinating university, the University of Tartu (first-year university), also Uppsala University (Sweden), Åbo Akademi University (Finland) and University Claude Bernard Lyon 1 (France) are involved as second-year and specialisation institutions.

The paper gives a comprehensive overview about the EACH programme, including a detailed overview of what EACH is, what kind of topics are taught during the first study-year at the University of Tartu, what is the nature of the different study-tracks (specialisation during second study-year either in Sweden, Finland or France), what extra activities, such as internship and winter school the EACH programme offers. The paper also gives an explanation on why it is necessary to have such a programme like EACH, and how to be a part of the EACH experience.

One section in the paper is dedicated to the impact of the EACH programme – with the four years that the programme has accepted students, it has reached a lot of countries and the employability rate of the graduates is almost 90%.

This Autumn, the fifth intake of EACH students is starting their studies at the University of Tartu, expanding the blue areas on the map presented above even more.

For more information on the EACH programme, please see the programme’s webpage and also the newly published paper.

Fluorescence spectroscopy course by EACH visiting scholar Todd Pagano

During Apr 22 to May 4 we had the pleasure to host visiting scholar, prof. Todd Pagano from the Rochester Institute of Technology (RIT), USA. He conducted, for the second time, a two week-intensive course Principles and applications of fluorescence spectroscopy.

In this course, students reviewed the principles of fluorescence spectroscopy, were introduced to the impact of photophysical phenomena on fluorescence data, and discussed new directions of fluorescence in analytical chemistry. Techniques in multidimensional fluorescence spectroscopy with chemometric analysis were highlighted, especially in the context of novel applications in environmental and related fields. The course consisted of lectures, seminars, tutorial sessions and two lab practicals. The latter were specifically set up for this course by prof. Pagano and were very much appreciated by students.

The first practical was about discovering the fundamental concepts of fluorescence (excitation and emission spectra, Stokes shift, Vavilov’s rule, fluorescence lifetime, etc). The second practical was about analysis of caffeine in beverages using salicylic acid as a fluorescent chemosensor. This analysis utilizes the ability of caffeine to quench the fluorescence of salicylic acid and introduces students to the fluorescence quenching, Stern-Volmer equation and inner filter effects.

Altogether 30 students (out of them 14 EACH students) participated in the course and their feedback was overwhelmingly positive.


Prof. Pagano is a passionate educator. He was the initiator of the Laboratory Science Technology program at Rochester Institute of Technology’s National Technical Institute for the Deaf, which is a unique science programme, specifically designed for deaf students. He was named “2012 U.S. Professor of the Year” by the Council for Advancement and Support of Education and the Carnegie Foundation for the Advancement of Teaching.


(Images: top left, group photo of prof. Pagano with course participants; right: prof. Pagano with students in lab)


EACH programme at the Sample Treatment 2018 Conference!

On Dec 3, 2018, Ivo Leito gave a presentation at the Sample Treatment 2018 conference (Caparica, Portugal) about the Excellence in Analytical Chemistry (EACH) Erasmus Mundus master’s programme that is coordinated by our group.

The focus of the talk was sample preparation and how is it included in the EACH programme. A key feature of the presentation was a question to the participants as for what else could/should the EACH programme contain in terms of sample preparation, especially keeping in mind emerging techniques. Another one was a call to come to teach at EACH as visiting scholar. During the subsequent coffee breaks a number of people approached Ivo and interesting ideas were proposed as to what to include into the programme’s set of covered sample preparation approaches (dialysis, different microextraction techniques, sonication, etc). Several people also expressed interest to contribute to the programme as visiting scholars.

Call of applications to the EACH visiting scholar scheme is constantly open at the EACH Visiting scholars page and submitting of application is non-binding, so it is encouraged also if you are not yet sure whether you will come.

We are thankful to all participants for their feedback and ideas!


Group seminar at Pühajärve

Ernesto giving his talk

From 24th to 25th of November our group had a traditional biannual seminar in Pühajärve Spa hotel. The seminar is a nice opportunity to learn about what the group members are doing and which challenges they are tackling. The presentations covered a broad domain of analytical chemistry from fundamental acid-base studies to bioanalyses and analyses of cultural heritage.

Ambient ionization and fluoroalcohols to improve bioanalysis

The first session was focusing on the bioanalytics. Max, a PhD fellow doing an internship in London right now, presented the results of drug analyses from a music festival. Next to strongly varying drug dose, the problem is the strongly varying dissolution of corresponding dose. Next two presentations presented by Rūta, a PhD fellow, and Krit, her undergraduate student introduced fluoroalcohols as novel LC eluent additives and their effect on retention mechanism and electrospray sensitivity. It was really interesting how strongly and unexpectedly differently some fluoroalcohols may change the retention mechanism.

The reliability of fluorescence measurement

The second session focused on acid-base and coordination chemistry. Alo, a PhD fellow, presented his improvements and challenges in the synthesis of bambusuril derivatives. Elisabeth, a master student, introduced 19F NMR measurements of pKa of fluorinated compounds in acetonitrile. Sigrid, a PhD fellow, gave a lecture on how to measure correct fluorescence spectra accounting all effects that may affect the spectra. She showed the importance of concentration and the inner filter effects correction on fluorescence spectrum. Andre, a PhD fellow, wrapped up the seminar with the presentation of his results in gas phase acidity measurements.

Did I get real cashmere scarf from the market?

The third session was focusing on the analysis of cultural heritage. Eliise, a PhD fellow, presented the comparison of four most applied derivatization procedures for analysis of binders in GC. Pilleriin, a PhD fellow, presented her results of textile analyses and a model developed  to classify unknown textiles using ATR-FT-IR spectroscopy. Markus, a master student, presented his work on coupling LC with nano-ESI FT-ICR-MS. Juhan, an undergraduate student, introduced his work on acid-base measurements of fluorophoric pH sensor molecules.

After inspiring presentation and fruitful discussions, we had a nice opportunity to relax in the spa and sauna. Additionally, group members discussed with Prof. Leito and Associate Prof. Herodes the SR-15 report from IPCC.

Is open science in terms of metadata really possible?

Next day was kicked off by Astrid, a PhD fellow, who compared the measurement of binding constants using isothermal calorimetry and NMR. Next, Piia, a PhD fellow, introduced her results on using the data from the literature to test, validate and improve the electrospray ionization efficiency prediction model. The take-home message from Piia’s presentation was the need for data integrity on results one is reporting and clear explanations on how one obtained these results. Additionally, a machine-readable format of the structure is a great help to simplify data mining from literature. Next, Jaanus, a PhD fellow introduced the results from a collaboration with a visiting PhD fellow Tingting Wang from DTU, Denmark. He showed the results of standard substance free quantification in the example of pesticides in food matrices. Ernesto, a PhD fellow, introduced his doctoral project on designing and describing the anionic derivatization reagents in LC/MS.

What’s causing this smell?

The second day was wrapped up by Associate Prof. Koit Herodes. He showed us a case study on the analysis of smell of ruined goods. Finally, he presented the current edition of validation software our group is developing to simplify and automate the validation in LC/MS analyses.

Thanks to all participants for interesting and inspiring presentation and for fruitful discussions.

UT analytical chemistry education activities at EcoBalt 2018 Conference

On Oct 26, 2018, Ivo Leito gave a presentation titled “Analytical chemistry education activities at University of Tartu” at the EcoBalt 2018 conference in Vilnius, Lithuania.

The presentation contains information about the online courses LC-MS Method Validation and Estimation of Measurement Uncertainty in Chemical Analysis, as well as the recently published tutorial reviews (Validation I, Validation II, LoD I, LoD II) that form the basis of the LC-MS Method Validation course.

The presentation also addresses the international master’s programmes Applied Measurement Science and Excellence in Analytical Chemistry at the University of Tartu.

The last part of the talk is devoted to the Eurachem 2018 General Assembly and Workshop that will take place in Tartu on May 20-21, 2018. The topic of the workshop is “Validation of targeted and non-targeted methods of analysis”.


Bachelor’s and Master’s Defences 2018

Traditionally, in the first half of June, our bachelor and master students defend their theses. This year there were 3 masters students and 2 bachelor students from our group. Here is how the students described their theses.

Alo Rüütel “Synthesis of bambusuril macrocycles and investigation of their binding properties”, master’s defence
In my master’s thesis, I synthesized bambusuril macrocycles. These receptor molecules are very potent anion binders. Usually, molecular receptors do not function in water because they are not able to bind target molecules with sufficient strength. Some bambusuril derivatives are able to function in aqueous media, which makes them a very special type of macrocyclic receptors. It is possible to use these molecules as ionophores for anion selective electrodes.

Ernesto de Jesus Zapata Flores “Determination of free diisocyanates in polyurethane foam”, master’s defence
My thesis focused on the test of a proposed method to analyze free diisocyanates in polyurethane foams for two reasons, by one side those compounds can represent a danger if care is not taken when the foam is used, and by the other side, new legislation is more aggressive against those compounds. The method is a simpler alternative to achieve the derivatization of diisocyanates.

Andre Leesment “Gas phase acidity measurements of superacids using FT-ICR method”, master’s defence

My master’s thesis was based on gas-phase acidity measurements of some very strong acids. Such strong acids are widely used in organic synthesis as reactants and/or catalysts. The anions of such acids exhibit high stability, which makes the valuable components of contemporary energy storing devices. The obtained results allow us to work on expanding the self-consistent gas-phase acidity scale with acids stronger than the ones experimentally measured so far.


Lisett Kiudorv “Quantitative analysis of clay components using ATR-FT-IR spectroscopy”, bachelor’s defence
The main purpose of my bachelor’s thesis was to develop a method that enables quantitative analysis of clays using ATR-FT-IR spectroscopy combined with the chemometric partial least squares method. The developed method is quick and easy to use and reduces the required sample size to around a milligram. The dramatic decrease in sample size makes it possible to analyse samples from archaeology and art. The method was then used to analyse six archaeological samples including one of the oldest potteries found in Estonia and an Egyptian pottery, which holds a bird’s mummy.

Elisabeth Parman “Determination of pKa values of fluorocompounds in water using 19F NMR”, bachelor’s defence
The main aim of my bachelor’s thesis was to determine pKa values of fluorocompounds in water using 19F NMR. This method is not particularly commonly used, but it can be used to verify or disconfirm values that have been measured with different methods, especially in cases where the measurements with other methods are problematic. For example, the purity and accurate concentration of the measured compound need to be concerned for most of the methods, but with 19F NMR it is not problematic.


Measurement uncertainty online course (MOOC) 2018 edition successfully finished!

Measurement_Uncertainty_MOOC_Successfully_FinishedOn May 14, 2018 the on-line course (MOOC) Estimation of measurement uncertainty in chemical analysis offered by University of Tartu finished successfully.
Eventually altogether 521 people registered (270 in 2014, 489 in 2015, 757 in 2016, 363 in 2017) from 76 countries (a number of participants joined after the start of the course). 358 participants actually started the course (i.e. tried at least one graded test at least once) and out of them 218 successfully completed the course (141 in 2014, 169 in 2015, 308 in 2016, 148 in 2017). The overall completion rate was 42% (52% in 2014, 34% in 2015, 40% in 2016, 41% in 2017). The completion rate of participants who started the studies was 61% (67% in 2014, 60% in 2015, 67% in 2016, 68% in 2017). The completion rates are nicely consistent over the last years and can be considered very good for a MOOC, especially one that has quite difficult calculation exercises, which need to be done correctly for completing the course.

The participants were very active and asked lots of questions. The questions were often very much to the point and addressed things that are really important to analysts in their everyday work. The course has several forums (general and by topic) and the overall number of posts to them during the course period reached almost 300 (!) (overall number of posts, both from participants and from teachers) and the forums are still active and posts are still coming in.

This active participation made teaching of this MOOC a great experience also for us, the teachers. The discussion threads gave a lot of added value to the course and some of them triggered making important modifications to the course materials, even during the course.

We want to thank all participants for helping to make this course a success!

We plan to repeat this course again in Spring 2019.


Another motivational group seminar took place on last weekend, 5-6th May

Traditional analytical chemistry group seminar was this time held in beautiful Voore Guest House on 5-6th of May. Despite the sunny and wonderful weather outside, a group of analytical chemists were pleased to stay inside to discuss research. Since many of our group members are going to defend their theses soon (PhD students Märt Lõkov and Sofja Tšepelevitš, master’s students Alo Rüütel and Andre Leesment, and bachelor’s students Elisabeth Parman and Lisett Kiudorv), their presentations were followed by many questions and fruitful discussions. Another PhD student, Max Hecht, joined us via Skype and gave us an interesting presentation about sponge spray while reminding that every chemist must face many problems and difficulties before gaining the expected results. Besides numerous analytical chemistry research-related presentations, our research fellow Dr. Riin Rebane, who is currently studying law, introduced us a world of law and talked about patent applications in Estonia. The whole seminar was finished with a gripping presentation about postdoctoral studies in the University of Helsinki by Dr. Hanno Evard.
In addition to the intense seminar, we were able to enjoy the beautiful nature and landscape of Vooremaa while taking a long walk in the village and discussing the day’s events in a hot sauna.