Estonian National Heritage Board award to Ackermann project!

The members of the Estonian Centre for Analytical Chemistry (including members from our group) have been partnering with art researchers for years in various interdisciplinary projects. One of the first projects for Rode altar in Niguliste church won many awards and the latest collaboration continues that tradition when on the 14th of October Estonian National Heritage Board awarded the team of Ackerman as the best research team!

Congratulations to everybody!

NB! The final exhibition will be in the Niguliste church and available for everybody starting on the 6th of November. It is a unique chance to see the sculptures from the same sculptor that have spent their time in various Estonian churches and never seen each other.

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).

We are happy to introduce – Dr. Ruta Hecht and Dr. Max Hecht

Today, on August 28, 2020, Ruta Hecht and Max Hecht defended successfully their PhD theses!

The dissertation by Ruta was titled “Novel eluent additives for LC-MS based bioanalytical methods”. In this thesis, novel fluoroalcoholic eluent additives that showed to have a positive influence on analyte ionisation in the MS source were studied. Additionally, two practical applications employing novel eluent additives were developed and validated for several pharmaceuticals. The two bioanalytical methods were used to obtain data for pharmacokinetic and pharmacodynamic studies in paediatric patients. Both methods reached exceptionally low limits of quantification, with minimal sample amount used due to the positive influence of novel eluent additives on analyte ionisation.

The PhD thesis by Max titled “Advances in the development of a point-of-care mass spectrometer test“. In this work, an on-site testing method was developed and evaluated for medical examination. For example, this method enabled to determine the concentration of an antibiotic and an opioid directly in blood, plasma, or urine in as little as 5 minutes.  Furthermore, traditional laboratory-based methods were developed. These included the diagnose of the rare MNGIE-disease and a 36-second test for the analysis of ecstasy tablets. To investigate potentially harmful drugs added to ecstasy tablets, a large panel of over 100 drugs was measured within a single analysis run on a miniaturised mass spectrometer. 

Congratulations to you both! We wish you all the best for the future!

Dr. Artur Gornischeff – PhD thesis on the study of ionization efficiencies and standard free quantification

On the 18th of August, 2020, Artur Gornischeff defended his PhD thesis titled Study of ionization efficiencies for derivatized compounds in LC/ESI/MS and their application for targeted analysis

In the thesis by Artur, a method that allowed to measure and evaluate the ionization efficiencies of important constituents (amino acids, biogenic amines) in different foodstuffs and beverages was developed. The developed useful method was used to estimate analyte concentrations without standard substances in different matrices (beer, wine, and tea). In addition, the effect of derivatization on ionization efficiencies and the problem of how to choose the suitable ion source and eluent components were addressed. One benefit of the overall results is the possibility to help with distinguishing counterfeit drinks from the original ones. 

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

 

 

 

 

 

Dr. Pilleriin Peets – PhD thesis on the analysis of textile fibres and dyes

Today, on August 25, 2020, Pilleriin Peets successfully defended her PhD thesis titled Development of instrumental methods for the analysis of textile fibres and dyes.

In the thesis by Pilleriin Peets, analytical methods using FT-IR spectroscopy in ATR and reflectance modes were developed for the determination of 16 different fibre types. Additionally, classification methods (discriminant analysis and random forest) were used for the classification of unknown fibres. For the dye analysis, analytical methods using various instrumental sets (HPLC with different mass analysers, MALDI- and ESI-FT-ICR-MS) were developed based on the analysis of seven natural red dyes

Based on these results, a large collection of standard spectra and chromatograms was collected and made available for scientists. The advantageous developed methods were used to analyse several cultural heritage samples from the University of Tartu Art Museum, Estonian National Museum, Conservation and Digitization Centre Kanut (Estonia) and private collections. 

Well done, Pilleriin! We wish you all the best for the future!

Design, synthesis and application of carbazole macrocycles in anion sensors

Our supramolecular analytical chemistry team has published an article (Beilstein J. Org. Chem. 2020, 16, 1901-1914) about developing carboxylate sensor prototypes that use macrocyclic carbazole receptors as ionophores.

Usually, reported research concludes with the demonstration of binding abilities of receptors and only suggests possible applications at a theoretical level. This work stands out from most publications by incorporating the entire workflow from receptor design to the characterisation of working sensor prototypes.

By involving this additional step, the team demonstrated the shortcoming of evaluating binding with just the receptor and analyte in solution. The predictions of selectivity can change considerably when measuring binding in an actual sensor membrane. This does not mean that such binding measurements would be obsolete, as the issue of binding anions selectively remains relevant in supramolecular chemistry.

The work was published in collaboration with the group of prof. Johan Bobacka at Åbo Akademi. The open access article was published in the Beilstein Journal of Chemistry thematic issue “Molecular Recognition” (in memory of Prof. Carsten Schmuck).

Symmetric Potentiometric Cells for the Measurement of Unified pH Values

Recently the UnipHied consortium published a new article – Symmetric Potentiometric Cells for the Measurement of Unified pH Values. Symmetry 2020, 12, 1150, where we compared the performance of different cells and instruments used to measure acidities on the unified pH scale (pHabs). The advantage of the unified pH scale is that it enables expressing the acidities of any systems – non-aqueous, solutions, colloidal systems, etc – via pHabsH2O values, which are directly comparable to the conventional pH values of the aqueous pH scale.

This is the first time unified acidities have been measured outside of our group. Nine partners from Europe – national metrology institutes and universities – have set up systems to measure pHabs and validated them with standard aqueous buffers.

The results show that the method is robust and does not depend on the cell nor the instrument (pH meter, potentiostat, or electrometer). The inherent symmetry of the cell design helps to reduce the experimental workload and improve the accuracy of the obtained results.

The next step is to measure unified acidities of non-aqueous systems, which could be used by routine laboratories to calibrate their pH electrodes.

The UnipHied project is funded from the EMPIR programme (project 17FUN09) co-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme.

A chemist with a Master’s degree in law

A member of our Analytical Chemistry group – Riin Rebane – achieved something rare for a chemist. On the 26th of May, she earned a Master’s degree in law!

Her studies combined both law and chemistry with a focus on intellectual property law. This was also the case for the topic of her Master’s thesis:  Interpretation of patent claims in Europe on the example of chemistry patents.

The aim of the thesis was to investigate how patent claims are interpreted during patent application expertise as well as in courts in the European Union and in the markets important to Europe. After investigating the practices of many countries, Riin concluded that patent claims in patent offices are interpreted quite similarly. However, it was observed from analyzing the practices of national courts that patent claim interpretation in courts is much more inconsistent and causes a lot of uncertainty for patent applicants and owners. For example, it is very likely that a patent approved by the patent offices can be revoked in court or even more confusing, a court in France may revoke, but a German court may not.

Congratulations to you, Riin! We are glad, that your hard work has paid off 😊.

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!

Our collection of acidity and basicity data in non-aqueous media has been updated!

The collections of experimental acidity and basicity data in non-aqueous media measured by our group are now up to date on our Chair of Analytical Chemistry webpage. 

Both tables include the compounds name, CAS number and SMILES code. The acidity collection contains 190 compounds, where the compounds available experimentally measured pKa in acetonitrile (MeCN) and pKip in 1,2-dichloroethane (DCE) are given. The pKa in DCE is calculated/estimated based on pKip value. 

The basicity data collection includes 353 compounds and their pKip in tetrahydrofuran (THF) and in DCE. The pKa values in MeCN were re-evaluated taking into account all (close to 700) measurements of 279 bases. Therefore, these pKa values can be considered the most reliable pKa values measured in MeCN available!