Development of on-line GC-MS and LC-MS methods based on Micro Extraction in Packed Sorbent (MEPS) for the OPCW proficiency test framework and on-site analysis

Project acronym:   MECWA FCUB CIA

Project type:   International Research Projects

Unique project identifier:   OPCW L/ICA/ICB/210502/17

Project is funded by:   Organisation for the prohibition of chemical weapons - OPCW (Hag, Netherlands)

Instituions where the research is conducted:

• University of Belgrade - Faculty of Chemistry (Belgrade, Serbia)
• Institute of Chemistry, Technology and Metallurgy (Belgrade, Serbia)
• Fakultet veterinarske medicine (Belgrade, Serbia)
• Farmaceutski fakultet (Belgrade, Serbia)
• Univerzitet u Hjustonu – Departman za hemiju (UH) (Hjuston, United States)

Project realization is scheduled from October 1, 2017 till April 30, 2021.

Project staff

Short description of the project

Fear of terrorism is growing and it becomes more frustrating, especially in present days after ISIS chemical weapons chief, captured by U.S. special forces, has revealed terrorists plan for mustard gas abuse in future attacks. It could be expected that the chemical weapon analysis (CWA) in official OPCW proficiency tests (PT) is going to be more demanding regarding sensitivity, sample amount, and chemical diversity (matrix and analytes). Today’s typical OPCW PT liquid samples are less than ten mL with concentration of target analytes as low as few ppm, and time frame 15 days from sample arrival to sending back report.

In this project proposal we hypothesize that Micro Extraction in Packed Sorbent (MEPS) could be a good alternative to today’s ROPs for OPCW PT, and good starting point for tomorrow’s demands. MEPS is relatively new method for sample preparation that could be performed directly on GC or LC instruments. Advantage of microextraction is that by skipping one step (SPE) in sample preparation and in combination with in-liner derivatization it becomes an automation method for water OPCW PT samples in GC based methods.

We intend to synthesize or obtain different agent degradation products and precursors (e.g. thiodiglycol, methylphosphonic acid, benzylic acid, pinacolyl alcohol, phosphonic esters from Schedule 2.B.04 group…) to prepare samples similar to OPCW PT samples, to develop and validate MEPS methods on Si, C8+SCX and C18 bins. Method development will be guided by NMR, GC-MS, and LC-MS analysis. Large volume injection will be tested in detail in order to achieve best limits of detection for each type of CW agents.

We expect that sample collection could be done manually by different types of MEPS syringes and then transferred to on-site laboratory for direct analysis. We will examine if MEPS syringes could be used for on-site sample collection.

In addition, one of the main goals of the project is training younger team members the way they could work independently in later stages.

Scientific results will be prepared for publication, and presented on advance courses at Faculty.

After the project ends we will continue developing MEPS application for CW metabolites from urine and blood samples, and try to employ MEPS analyses for food and pharma industry. Finally we are confident that proposed MEPS project will be sustainable in the future.

Short description of research results

The MECWA CIA FCUB project developed new qualitative sample preparation methods for GC and LC related techniques based on Micro Extraction in Packed Sorbent (MEPS) to support the  OPCW  proficiency  tests  and  on-site  sample  collection  and  CW  analysis.  It  is clearly demonstrated that MEPS could achieve low ppb levels of detection limits for CWC related chemicals in OPCW  PT similar  samples eveen in combination with GC-MS with single quadrupole. It is also demostrated that MESP bin could use as sample collector for organic CW samples and analysed up to minimum trheee weeks after collection of sample store at room temperature and ambient lights.  Automation of MEPS sample preparation is very useful technique, and it is a big step forward to green chemical analysis.

Representative references

RSC Twitter Conference 2019 (5.mart 2019)

https://twitter.com/ljubaw78/status/1102861810657607680?s=20

https://www.opcw.org/media-centre/news/2016/05/eastern-european-states-pledge-support-opcw-education-and-outreach