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.

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.  

 

 

 

 

 

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!