Development and implementation of "green" methods for determining organic toxicants in soils

Project of the Ministry of Education and Science of the Republic of Kazakhstan
3661/GF4

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Relevance of the project:

The main way to ensure environmental safety is continuous monitoring and control of the content of toxic compounds in environmental objects. Soil is the most polluted and complex object for analysis. Determining organic pollutants in soil requires lengthy and "dirty" sample preparation using toxic organic solvents.
Currently, green analytical chemistry, a branch of green chemistry aimed at developing environmentally safe analysis methods, has become widespread. The most promising and "green" sample preparation method is solid-phase microextraction (SPME), based on the extraction of analytes from the gas phase above the soil or water-soil suspension, allowing the combination of extraction, concentration, and purification in one stage.
Based on this method, hundreds of techniques have been developed for determining organic pollutants in environmental objects and food products. However, when using SPME, the greatest challenge is the quantitative determination of analytes in solid samples. The mechanical composition and moisture content of the sample, as well as the concentration of organic carbon, significantly affect the extraction efficiency and analyte response.
To minimize and control the matrix effect, scientists have proposed several methods: adding excess water to eliminate the influence of moisture; preliminary extraction with an organic solvent followed by its evaporation and water addition; complete extraction with a cold fiber. However, using these methods leads to a significant reduction in method sensitivity, the use of toxic solvents, or a substantial increase in cost and complexity of the analysis.
This project proposes to control the matrix effect using internal standard and spiking methods without additional sample modification. The project will address the problem of long equilibration of introduced standards throughout the sample volume. A methodology for optimizing SPME-based techniques will be developed, aimed at achieving maximum accuracy.

Project goal:

develop and implement new "green" methods for determining organic toxicants in soils.

Project objectives:

  1. Improvement of solid-phase microextraction methodology for the determination of organic pollutants in soils.
  2. Development of four new methods for the quantitative determination of the following organic toxicants in soil samples based on solid-phase microextraction: 1-methyl-1H-1,2,4-triazole; unsymmetrical dimethylhydrazine (with derivatization), phenol; aromatic hydrocarbons.
  3. Testing and implementation of developed methods for soil analysis collected in Kazakhstan.

Used methods:

  • Gas chromatography with mass spectrometric detection
  • Solid-phase microextraction

Advantages of the developed methods over classical ones:

  • Significantly lower cost per sample analysis (up to 10 times) due to minimal material costs and automation;
  • Practically no emissions of toxic compounds into the environment and toxic waste.

To potential users of developments:

If you are interested in using the developed methods, please contact the project manager Bulat Nurlanovich Kenessov at bkenesov@cfhma.kz.

Publications on the project:
Articles in international journals:

  1. Yegemova S., Bakaikina N.V., Kenessov B., Koziel J., Nauryzbayev M., 2015. Determination of 1-methyl-1H-1,2,4-triazole in soils contaminated by rocket fuel using solid-phase microextraction, isotope dilution and gas chromatography - mass spectrometry. Talanta 143, 226-233. (IF=4.162, first quartile in the "Chemistry, Analytical" category)
  2. Zhubatov Z.K., Kenessov B., Bakaikina N.V., Bimaganbetova A.O., Akynbayev N., Bakhytkyzy I., 2016. Fast determination of 1-methyl-1H-1,2,4-triazole in soils contaminated by rocket fuel using solvent extraction, isotope dilution and GC-MS. Chromatographia 79, 491-499. (IF=1.402, third quartile in the category "Chemistry, Analytical")
  3. Kenessov B., Koziel J., Bakaikina N.V., Orazbayeva D., 2016. Perspectives and challenges of on-site quantification of organic pollutants in soils using solid-phase microextraction. TrAC Trends in Analytical Chemistry 85B, 111-122. (IF = 8.442, first quartile in the "Chemistry, Analytical" category)
  4. Orazbayeva D., Kenessov B., Koziel J.A., Nassyrova D., Lyabukhova N.V., 2017, Quantification of BTEX in soil by headspace SPME-GC-MS using combined standard addition and internal standard calibration. Chromatographia 80, 1249-1256. (IF=1.402, third quartile in the category "Chemistry, Analytical")
  5. Bakaikina N.V., Kenessov B., Ul'yanovskii N.V., Kosyakov D.S., 2018. Quantification of transformation products of rocket fuel unsymmetrical dimethylhydrazine in soils using SPME and GC-MS. Talanta 184, 332-337. (IF = 4.162, first quartile in the "Chemistry, Analytical" category)
  6. Orazbayeva D., Kenessov B., Psillakis E., Nassyrova D., Bektassov M. Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted headspace solid-phase microextraction. Journal of Chromatography A 1555, 30-46. (IF = 3.981, first quartile in the "Chemistry, Analytical" category).

Conference abstracts:

  1. Egemova S.S., Bakaikina N.V., Kenessov B.N., 2015. Quantitative determination of 1-methyl-1H-1,2,4-triazole in soils at rocket carrier fall sites by solid-phase microextraction combined with gas chromatography-mass spectrometry. Abstracts of the All-Russian Conference "Theory and Practice of Chromatography", Samara, Russia. p.222.
  2. Bakaikina N.V., Yegemova S.S., Kenessov B.N., 2015. Study and minimization of matrix effect during determination of 1-methyl-1H-1,2,4-triazole by headspace solid-phase microextraction and GC-MS in soils contaminated by unsymmetrical dimethylhydrazine rocket fuel residuals. Abstracts of the International conference “Mendeleev-2015”, Saint Petersburg, Russia. P.370.
  3. Bakaikina N.V., Yegemova S.S., Kenessov B., 2015. Fast quantification of transformation products of rocket fuel unsymmetrical dimethylhydrazine in soil using solid-phase microextraction and GC-MS. Abstracts of the International Chemical Congress "Pacifichem-2015". ANYL 664.
  4. Orazbayeva D., Karatayeva U., Kenessov B., Koziel J.A., 2016. Quantification of BTEX in soil by SPME-GC-MS using standard addition and internal standard approaches. Abstracts of 18th International Symposium on Advances in Extraction Technologies & 22nd International Symposium on Separation Sciences, Torun, Poland. P.151.
  5. Bakaikina N.V., Kenessov B.N., Ulyanovskiy N.V., Kosyakov D.S., Pokryshkin S.A., 2017. Determination of transformation products of unsymmetrical dimethylhydrazine in soil by HS-SPME-GC-MS/MS. Abstracts of the All-Russian Conference "Analytical Chromatography and Capillary Electrophoresis", Tuapse, Russia. P.194.
  6. Orazbayeva D., Kenessov B., Nassyrova D., Lyabukhova N., Bektassov M., Psillakis E., 2017. Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted HSSPME. Abstracts of 19th International Symposium on Advances in Extraction Technologies, Santiago de Compostela, Spain. P.354.

Interactive online lectures:

  1. Kenessov B.N., Tukhmetova D., Shakeshev M. Introduction to Solid Phase Microextraction (in English and Russian)
  2. Kenessov B.N., Orazbayeva D.S., Umirbekova Zh. Quantitative chemical analysis using solid-phase microextraction (in English and Russian)

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