Congratulations on the ERC Consolidator Grant!

We are delighted to announce that the prestigious ERC Consolidator Grant 2023 was awarded to a former member of our Analytical Chemistry group, Associate Professor Anneli Kruve at Stockholm University!

Anneli Kruve

The European Research Council (ERC) Consolidator Grant is aimed to support early-career researchers to consolidate their own independent research team or program over the next five years. We are very proud that this year one of the awardees was Anneli Kruve, Associate Professor at Stockholm University and head of the Mass Spectrometry Laboratory. In her research, she combines analytical chemistry with modeling and machine learning. The goal of the ERC funding is to support the research of her group on developing broader and more accurate methods to characterize and measure toxic chemicals in environmental samples. 

Only a few percent of chemicals that cause the toxic activity of environmental samples are currently known. In this project, Anneli and her group will combine high-resolution mass spectrometry and machine learning to find novel toxic chemical structures, which enables focusing the toxicity research on chemicals that truly matter. Understanding the emission and transformation processes of toxic chemicals is a necessary step to decrease the chemical risks in the environment. 

More information about the research performed by Anneli’s group can be found on the Kruve lab webpage

LC-MS Method Validation web course: 1013 participants from 109 countries!

Number of participants and countries updated on 22.11.2023!

On Tuesday, November 21, 2023 the web course LC-MS Method Validation was launched for the fifth time as a MOOC (Massive Online Open Course). There are 973 1013 registered participants (the first time ever over 1000) from 107 109 countries, ranging from Chile to China and from Australia to Iceland. And the number is still growing. The image below shows the countries where the participants come from.

This is a practice-oriented on-line course on validation of analytical methods, specifically using LC-MS as technique. The course introduces the main concepts and mathematical apparatus of validation, covers the most important method performance parameters and ways of estimating them. The LC-MS validation course is delivered by a team of 7 teachers, each with their own specific area of competence. This way it is expected to offer the best possible knowledge in all the different subtopics of analytical method validation.

The full set of course materials is accessible from the web page https://sisu.ut.ee/lcms_method_validation/. The course materials include videos, schemes, calculation files and numerous self-tests (among them also full-fledged calculation exercises). In order to pass the course, the registered participants have to take all tests and get higher than 50% score from each of them. These tests are available to registered participants via the Moodle e-learning platform. Participants who successfully pass the course will get a certificate from the University of Tartu.

Dr. Ernesto de Jesus Zapata Flores – PhD thesis on LC-MS derivatization reagents

Last Wednesday, August 30th, 2023, a moment that marks the culmination of years of hard work and determination of Ernesto de Jesus Zapata Flores – an AMS alumnus. He successfully defended his PhD thesis titled Derivatization Reagents used in negative mode electrospray LC-MS. The opponent was Associate Professor Jeffrey Hawkes from the University of Uppsala, Sweden.

In the vast application of derivatization reagents in RPLC-UV and RPLC-MS positive mode, Ernesto’s thesis delved into the question: What about LC-MS negative mode? Why don’t we compare both modes and see the best of both worlds?

Firstly, the thesis has been inspired by DEEMM – a commercial reagent – which also was one of the earliest reagents studied in our department. The comparison of the ionization mode in the determination of free amino acids in beers showed that (1) the matrix effects were less severe in the negative mode.

Later on, the method applying two azobenzene-based reagents, which were called AzoB and AzoC  (synthesized in our lab), has been fully developed specifically for LC-QqQ. The “gourmet” part that Ernesto has brought to the table of the analytical chemistry community was the study of (2) MS/MS fragmentations of all three reagents with different amino compounds in both ionization modes.

Moreover, his thesis has demonstrated comprehensive research about (3) optimization for the derivatization process and the ion source, (4) the confirmation of reaction yields, and (5) the correlation between ionization efficiency and LOD/LOQ of derivatives. Finally, applications of the validated method (7) for real-world samples (different beverages: beers, Kali, juices) and (8) neutral loss scan have been showcased.

Alongside the road, (9) side reactions managed to be worth some of his sweat and tears. At the end of his PhD journey, he (10) evaluated an identification tool using the transition of derivatives in both MS polarities.

10 out of 10 – that should be given for Ernesto’s dedication on the road to becoming an expert in LC-MS derivatization. Congratulations, Ernesto! We eagerly await your next academic steps. Hopefully, all your goals will be achieved.

LC-MS Validation online course 7th run has finished!

On February 10, 2023 the on-line course (MOOC) LC-MS Method Validation offered by the University of Tartu finished successfully.

Eventually, altogether 903 people registered from 104 countries. Less than half, 376 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. The overall completion rate was 24%. The completion rate of participants who started the studies was 58%. The completion rates of active participants (i.e. who started the course) seems to have stabilized not too far from 60%, which can be considered good. However, the overall completion rate is still in decline (although there is no statistically significant difference between the 25% and 24% of the last two editions). In any case, there is some food for thought for us on how we could improve the overall completion rate…

At the same time, those participants who actually took part in the course, 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 during the course period the overall number of forum posts was above 400 (!) (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. Importantly, thanks to active participants, several mistakes were found and corrected in the course materials. As a result, the overall quality of the course improved.

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

We plan to repeat this course again in Autumn 2023.

On-line LC-MS Method Validation Course 2022-2023: Registration is open!

We are glad to announce that the seventh edition of the online course LC-MS Method Validation is open for registration (here)! The course will be offered as a Massive Open On-line Course (MOOC) during Nov 22, 2022 – Feb 03, 2023.

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 chromatography practitioners 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. More information about the course can be found in Course introduction page.

Participation in the course is free of charge. Receiving 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 web by anyone who wishes to improve the knowledge and skills in analytical method validation (especially when using LC-ESI-MS).

We are also glad to announce, that the course has been added into the BIPM (Bureau International des Poids et Mesures) e-learning platform. The BIPM is the most important international metrology organization established by the Metre Convention, through which Member States act together on matters related to measurement science and measurement standards. BIPM is also the home of the International System of Units (SI) and the international reference time scale (UTC). The Institute of Chemistry of University of Tartu is a designated institute by the BIPM since 2010.

We are sure that being on this platform, will enable more people to find our course.

LC-MS Validation online course 6th run has finished!

On February 11, 2022 the on-line course (MOOC) LC-MS Method Validation offered by the University of Tartu finished successfully.

Eventually, altogether 850 people registered from 97 countries. Less than half, 380 participants actually started the course (i.e. tried at least one graded test at least once) and out of them 209 successfully completed the course. The overall completion rate was 25%. The completion rate of participants who started the studies was 55%. These completion rates are lower than we usually have. So, here is some food for thought for us on how we could improve the success rate…

At the same time, those participants who actually took part in the course, 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 during the course period the overall number of forum posts was above 200 (!) (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 Autumn 2022.

LC-MS Method Validation web course: 854 participants from 97 countries!

On Tuesday, November 23, 2021 the web course LC-MS Method Validation was launched for the sixth time as a MOOC (Massive Online Open Course).

There are 854 registered participants (the largest number ever in this course) from 97 countries. Both numbers are the largest we have had! The countries range from Philippines to Paraguay and from Sweden to Sri Lanka. Image on the left shows the countries where the participants come from.

This is a practice-oriented on-line course on validation of analytical methods, specifically using LC-MS as technique. The course introduces the main concepts and mathematical apparatus of validation, covers the most important method performance parameters and ways of estimating them. The LC-MS validation course is delivered by a team of 8 teachers, each with their own specific area of competence. This way it is expected to offer the best possible knowledge in all the different subtopics of analytical method validation.

The full set of course materials is accessible from the web page https://sisu.ut.ee/lcms_method_validation/. The course materials include videos, schemes, calculation files and numerous self-tests (among them also full-fledged calculation exercises). In order to pass the course the registered participants have to take all tests and get higher than 50% score from each of them. These tests are available to registered participants via the Moodle e-learning platform. Participants who successfully pass the course will get a certificate from the University of Tartu.

Derivatization-targeted analysis of amino compounds in plant extracts by LC-MS/MS

In the recently published paper including the members of our Analytical Chemistry Chair, a method was developed to detect amino compounds with diethyl ethoxymethylenemalonate (DEEMM) derivatization in neutral loss scan mode by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Amino compounds react with DEEMM, and the derivatives lose a neutral ethanol molecule [M+H-46]+ from the parent ion upon collision-induced dissociation (CID) fragmentation. Therefore, it is possible to employ neutral loss scan (NLS) mode of the triple quadrupole mass analyzer.

The first part of the work was dedicated to the development of the method, such as testing different solvents and quenching reagents in order to obtain a cleaner chromatographic profile. Hydroxylamine was chosen as the quenching reagent, considering the retention time of its DEEMM-derivative and its solubility in the solvent employed (0.1 M HCl in 30% methanol).

Finally, the developed method was applied to an extract from the plant species Carduus nutans subsp. macrocephalus (Desf.) Nyman, in which 18 amino acids and 3 biogenic amines were identified for the first time in this plant species. The method can be applied to different matrices for the detection of known and unknown amino compounds.

Here you can find the 50-day free access to the article.

Dr. Merit Oss, PhD thesis on the ionization efficiency in ESI

On the 24th of August, 2021, Merit Oss successfully defended her PhD thesis titled “Ionization efficiency in electrospray ionization source and its relations to compounds’ physico-chemical properties” 

The thesis by Merit revolves around ionization efficiency in electrospray ionization (ESI) MS. The main aim was to gain a better understanding of the relations between different molecular properties of compounds and the signal intensities of their ions in ESI-MS. During this study, a large number of ionization efficiency values were obtained. Eleven molecular parameters were taken into account for estimating their importance for evaluating the compound’s ionization efficiency in ESI. It was concluded that in the studied solvent system, a compound’s ionization in the ESI source is determined by its basicity, molecular size, and hydrophobicity/lipophilicity. The results showed that the obtained models for estimating compounds’ ionization efficiency can be used for approximate prediction. 

Congratulations, Merit! We wish you all the best for your future. 

 

LC-MS Method Validation online course finished with 28% completion rate!

Altogether 791 people were registered from 86 countries. 338 participants actually started the course (i.e. tried at least one graded test at least once) and out of them 221 successfully completed the course. The overall completion rate was 28%. The completion rate of participants who actually started the studies was 65%. All statistics during the five years can be found in the table below.

Year No of registrations No of countries Active participants Completion rate: Overall Completion rate: Participants who started studies
2017 303 61 224 55% 75%
2018 424 71 236 37% 67%
2019 426 70 227 29% 55%
2020 515 77 267 31% 60%
2021 791 86 338 28% 65%

Both the overall completion rate, as well as the completion rate of those participants who actually started the course have stabilized. The latter completion rate can be considered very good by any measure. As has been the usual case with our online courses, the questions from the participants were often very interesting, often addressed things that are really important to analysts in their everyday work. Such discussions made teaching this course a great experience also for us, the teachers!

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

We plan to repeat this course again in Autumn-Winter 2021-2022.