Optimization of the sample preparation procedure in the determination of y-hexachlorocyclohexane in water by gas chromatography
https://doi.org/10.26896/1028-6861-2023-89-3-25-30
Abstract
A high toxicity of organochlorine compounds, even present in trace amounts in food products, leads to increased requirements for the accuracy of chemical analysis in food safety control. The interstate standard GOST 31858-2012 was taken as a basis for this study. We have improved the method of sample preparation of drinking water for the determination of residual amounts of y-hexachlorocyclohexane (y-HCCH) by gas chromatography with an electron capture detector. Strictly following the instructions of the standard, we failed to obtain the value of the recovery factor of 94% prescribed by GOST for y-HCCH. In this regard, we proposed to use higher-boiling re-heptane instead of re-hexane as an extractant to reduce losses at the stage of sample preparation, and to use sodium chloride instead of ethyl alcohol prescribed by GOST to break the emulsion formed during the extraction of water with hexane. The volume of the analyzed sample, the mass of sodium chloride, the volume of the extragent, and the extraction time were optimized. The use of sodium chloride is shown to provide total emulsion breakage in 100% of experiments and to increase the recovery of pesticides with a concentration of 22 pg/liter from 77 to 96% with a relative standard deviation of 2%. Replacing the extragent with re-heptane led to an increase in the recovery of Y-HCCH to 98% with a relative standard deviation of 1%. It is shown that at a lower concentration of the pesticide, the recovery rate is 98 - 100 %. An increase in the concentration of y-HCCH to 45 pg/liter leads to a sharp decrease in the recovery degree. The proposed method can be considered as an improved method of liquid-liquid extraction with excellent extraction of the pesticide from the aqueous matrix.
About the Authors
D. E. Musabirov
Ufa Research Institute of Occupational Medicine and Human Ecology; Bashkir State University
Russian Federation
Russian Federation
Dmitry E. Musabirov
450106, Ufa, ul. Kuvykina, 94
R. A. Daukaev
Ufa Research Institute of Occupational Medicine and Human Ecology
Russian Federation
Russian Federation
Rustem A. Daukaev
450106, Ufa, ul. Kuvykina, 94
G. R. Allayarova
Ufa Research Institute of Occupational Medicine and Human Ecology
Russian Federation
Russian Federation
Guzel R. Allayarova
450106, Ufa, ul. Kuvykina, 94
E. E. Zelenkovskaya
Ufa Research Institute of Occupational Medicine and Human Ecology
Russian Federation
Russian Federation
Evgenia E. Zelenkovskaya
450106, Ufa, ul. Kuvykina, 94
V. Y. Guskov
Bashkir State University
Russian Federation
Russian Federation
Vladimir Yu. Guskov
Ufa
References
1. Drugov Yu. S., Zenkevich I. G., Rodin A. A. Gas chromatographic identification of air, water, soil and biological media pollution: A practical guide. — Moscow: Binom. Laboratoriya znanii, 2005. — 752 p. [in Russian].
2. Briggs D. J., Courtney E M. Agriculture and Environment: The Physical Geography of Temperature Agricultural Systems. — London - New York: Longman, 1985. E 33.
3. Manahan S. E. Environmental Chemistry. — Chelsea, MI: Lewis Publishers, 1990. — 612 p.
4. Hennion M.-C, Pichon V, Barcelo D. Surface water analysis (trace-organic contaminants) and EC regulations / Trends Anal. Chem. 1994. Vol. 13. N 9. E 361 - 372. DOI:10.1016/0165-9936(94)85007-0
5. Technical Regulations of the Eurasian Economic Union "On the safety of packaged drinking water, including natural mineral water" (TR EAEU 044/2017). https://docs.cntd.ru/document/456090353 (accessed October 10, 2022) [in Russian].
6. Dogheim S. M., Mohamed E. Z., Gad Alia S. A., et al. Monitoring of pesticide residues in human milk, soil, water and food samples collected from Kafr El-Zayat Governorate / J. AOAC Int. 1996. Vol. 79. N 1. E 111 - 116. DOI:10.1093/jaoac/79.1.111
7. Brito N. M., Navickiene S., Polese L., et al. Determination of pesticide residues in coconut water by liquid-liquid extraction and gas chromatography with electron-capture plus thermionic specific detection and solid-phase extraction and high-performance liquid chromatography with ultraviolet detection / J. Chromatogr. A. 2002. Vol. 957. N 2. E 201 - 209. DOI:10.1016/S0021-9673(02)00351-5
8. Soler C, Manes J., Pico Y. Liquid chromatography-electrospray quadrupole ion-trap mass spectrometry of nine pesticides in fruits / J. Chromatogr. A. 2004. Vol. 1048. N 1. E 41 - 49. DOI:10.1016/j.chroma.2004.07.023
9. Nardelli V., Palermo C, Centonze D. Rapid multiresidue extraction method of organochlorinated pesticides from fish feed / J. Chromatogr. A. 2004. Vol. 1034. N 1 - 2. E 33 - 40. DOI:10.1016/j.chroma.2004.02.018
10. Lopez F. J., Beltran J., Forcada M., Hernandez F. Comparison of simplified methods for pesticide residue analysis. Use of large-volume injection in capillary gas chromatography / J. Chromatogr. A. 1998. Vol. 823. N 1 - 2. E 25 - 33. DOI:10.1016/S0021-9673(98)00393-8
11. Tahboub Y. R., Zaater M. F, Al-Talla Z. A. Determination of the limits of identification and quantitation of selected organochlorine and organophosphorous pesticide residues in surface water by full-scan gas chromatography/mass spectrometry / J. Chromatogr. A. 2005. Vol. 1098. N 1 - 2. E 150 - 155. DOI:10.1016/j.chroma.2005.08.064
12. GOST 31858-2012. Drinking water. Method for determining the content of organochlorine pesticides by gas-liquid chromatography. sian. Moscow: Standartinform, 2014. — 11 p.
13. Concha-Grana E., Fernandez-Martinez G., Fernandez-Vfflarrenaga V, et al. A study of large-volume on-column injection GC-ECD for the ultratrace analysis of organochlorine pesticides in water / Talanta. 2009. Vol. 78. N 3. E 764 - 771. DOI:10.1016/j.talanta.2008.12.043
14. Quayle W. C., Jepson I., Fowlis I. A. Simultaneous quantitation of sixteen organochlorine pesticides in drinking waters using automated solid-phase extraction, high-volume injection, high-resolution gas chromatography / J. Chromatogr. A. 1997. Vol. 773. N 1 - 2. E 271 - 276. DOI:10.1016/S0021-9673(97)00190-8
15. Rezaee M., Assadi Y., Milani Hosseini M. R., et al. Determination of organic compounds in water using dispersive liquid-liquid microextraction / J. Chromatogr. A. 2006. Vol. 1116. N 1 - 2. E 1 - 99. DOI:10.1016/j.chroma.2006.03.007
16. Basheer C., Lee H. K., Obbard J. P. Determination of organochlorine pesticides in seawater using liquid-phase hollow fibre membrane microextraction and gas chromatographymass spectrometry / J. Chromatogr. A. 2002. Vol. 968. N 1 - 2. E 191 - 199. DOI:10.1016/S0021-9673(02)00793-8
Review
For citations:
Musabirov D.E., Daukaev R.A., Allayarova G.R., Zelenkovskaya E.E., Guskov V.Y. Optimization of the sample preparation procedure in the determination of y-hexachlorocyclohexane in water by gas chromatography. Industrial laboratory. Diagnostics of materials. 2023;89(3):25-30. (In Russ.) https://doi.org/10.26896/1028-6861-2023-89-3-25-30
Views:
321
Email this article 