Validation of method for determination of organochlorine pesticides in grain and flour by GC-MS/MS using QuEChERS sample preparation
Abstract
A method for the determination of 9 organochlorine pesticides (a-HCH, β-HCH, γ-HCH, DDE, DDD, DDT, aldrin, heptachlor, hexachlorobenzene) in grain and flour has been validated using GC-MS/MS. The optimal conditions for chromatography and sample preparation based on the QuEChERS method have been selected. The degree of pesticide extraction ranged from 88 to 119%. The range of determined pesticide concentrations was evaluated at 0,002 – 0,020 mg/kg. The relative standard deviation of the analysis results did not exceed 16%. The LOD (limit of detection) values were 0,0003 – 0,0011 mg/kg, while the LOQ (limit of quantification) values were 0,0011 – 0,0034 mg/kg.
References
Kiwango, P.A., Kassim, N., & Kimanya, M.E. (2020). Household vegetable processing practices influencing occurrence of pesticide residues in ready-to-eat vegetables. Journal of Food Safety, 40(1). https://doi.org/10.1111/jfs.12737
Tarmure, S., Alexescu, T.G., Orasan, O., Negrean, V., Sitar-Taut, A.V., Coste, S.C., & Todea, D.A. (2020) Influence of pesticides on respiratory pathology - a literature review. Annals of Agricultural and Environmental Medicine, 27(2), 194–200. https://doi.org/10.26444/aaem/121899
Jirsova, S. (2018) The effect of polychlorinated biphenyls and organochlorinated pesticides on human reproduction. Ceska Gynekologie-Czech Gynaecology, 83(5), 380–384.
CU TR 015/2011. Аbout grain safety. Minsk, 2013, 26 p. (in Russ.).
Li, G. J., Zhang, X., Liu, T. T., Fan, H. X., Liu, H. C., Li, S. Y., Wang, D. W., & Ding, L. (2021). Dynamic microwave-assisted extraction combined with liquid phase microextraction based on the solidification of a floating drop for the analysis of organochlorine pesticides in grains followed by GC. Food Science and Human Wellness, 10(3), 375–382. https://doi.org/10.1016/j.fshw.2021.02.029
Dimitrova, R.T., Stoykova, II, Yankovska-Stefanova, T.T., Yaneva, S.A., & Stoyanchev, T.T. (2018). Development of analytical method for determination of organochlorine pesticides residues in meat by GC-ECD. Revue De Medecine Veterinaire, 169(4–6), 77–86.
Wang, Y., Ye, Q., Yu, M.H., Zhang, X.J., & Deng, C.H. (2020). Sulfonic acid-based metal organic framework functionalized magnetic nanocomposite combined with gas chromatography-electron capture detector for extraction and determination of organochlorine. Chinese Chemical Letters, 31(7), 1843–1846. https://doi.org/10.1016/j.cclet.2020.02.054
Martel, A.C., Mangoni, P., & Gastaldi-Thiery, C. (2018). Validation of a multiresidue method for the determination of pesticides in honeybees by gas chromatography. International Journal of Environmental Analytical Chemistry, 98(1), 31–44. https://doi.org/10.1080/03067319.2018.1426754
Mardani, A., Mogaddam M.R.A., Farajzadeh, M.A., Mohebbi, A., Nemati, M., & Torbati, M. (2020). A three-phase solvent extraction system combined with deep eutectic solvent-based dispersive liquid-liquid microextraction for extraction of some organochlorine pesticides in cocoa samples prior to gas chromatography with electron capture detection. Journal of Separation Science, 43(18), 3674–3682. https://doi.org/10.1002/jssc.202000507
Asati, A., Satyanarayana, G.N.V., Srivastava, V.T., & Patel, D.K. (2018). Determination of organochlorine compounds in fish liver by ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of organic droplet coupled with gas chromatography-electron capture detection. Journal of Chromatography A, 1561, 20–27. https://doi.org/10.1016/j.chroma.2018.05.035
Sun, P., Cui, Y.H., Yan, R., & Lian, Y.F. (2021). Determination of organochlorine pesticides in water using GC combined with dispersive solid-phase extraction with single-walled carbon nanotubes. Acta Chromatographica, 33(2), 202–207. https://doi.org/10.1556/1326.2020.00840
Rezaei, F., & Hosseini, M.-R. M. (2011). New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid–liquid extraction for the determination of some organochlorinated pesticides in fish. Analytica chimica acta, 702(2), 274–279. https://doi.org/10.1016/j.aca.2011.06.008
Kaur, R., Rani, S., Malik, A.K., Kabir, A., Furton, K.G., & Samanidou, V.F. (2019). Rapid Monitoring of Organochlorine Pesticide Residues in Various Fruit Juices and Water Samples Using Fabric Phase Sorptive Extraction and Gas Chromatography-Mass Spectrometry. Molecules, 24(6). https://doi.org/10.3390/molecules24061013
Phosiri, P., Burakham, R. (2021). Deep eutectic solvent-modified mixed iron hydroxide-silica: Application in magnetic solid-phase extraction for enrichment of organochlorine pesticides prior to GC-MS analysis. Journal of Separation Science, 44(19), 3636–3645. https://doi.org/10.1002/jssc.202100329
Li, J., Li, H., Zhang, W.J., Wang, Y.B., Su, Q., Wu,L. (2018). Hollow Fiber-Stir Bar Sorptive Extraction and Gas Chromatography-Mass Spectrometry for Determination of Organochlorine Pesticide Residues in Environmental and Food Matrices. Food Analytical Methods, 11(3), 883–891. https://doi.org/10.1007/s12161-017-1053-5
Szarka, A., Bucikova, K., Kostic, I., & Hrouzkova, S. (2020). Development of a Multiresidue QuEChERS-DLLME-Fast GC-MS Method for Determination of Selected Pesticides in Yogurt Samples. Food Analytical Methods, 13(10), 1829–1841. https://doi.org/10.1007/s12161-020-01809-0
Ozdemir, C., Ozdemir, S., Oz, E., & Oz, F. (2019). Determination of organochlorine pesticide residues in pasteurized and sterilized milk using QuEChERS sample preparation followed by gas chromatography-mass spectrometry. Journal of Food Processing and Preservation, 43(11). https://doi.org/10.1111/jfpp.14173
Kang, H.S., Kim, M., Kim, E.J., & Choe, W.J. (2020). Determination of 66 pesticide residues in livestock products using QuEChERS and GC-MS/MS. Food Science and Biotechnology, 29(11), 1573–1586. https://doi.org/10.1007/s10068-020-00798-4
Mandal, S., Poi, R., Bhattacharyya, S., Ansary, I., Roy, S.D., Hazra, D.K., & Karmakar, R. (2020). Multiclass Multipesticide Residue Analysis in Fish Matrix by a Modified QuEChERS Method Using Gas Chromatography with Mass Spectrometric Determination. Journal of Aoac International, 103(1), 62–67. https://doi.org/10.5740/jaoacint.19-0205
Mandal, S., Poi, R., Ansary, I., Hazra, D. K., Bhattacharyya, S., & Karmakar, R. (2020). Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC-MS and LC-MS/MS and its application in real sample analysis. Sn Applied Sciences, 2(2). https://doi.org/10.1007/s42452-020-1990-2
Ahmad, Y.H., & Khulod, I.H. (2020). Development and methods of validation for measurement of pesticides in muscle tissue using gas chromatography based modified analytical QuEChERS approach. Applied Ecology and Environmental Research, 18(1), 275–288. http://dx.doi.org/10.15666/aeer/1801_275288
Salemi, A., Khaleghifar, N., Mirikaram, N. (2019). Optimization and comparison of membrane-protected micro-solid-phase extraction coupled with dispersive liquid-liquid microextraction for organochlorine pesticides using three different sorbents. Microchemical Journal, 144, 215–220. https://doi.org/10.1016/j.microc.2018.09.011
Wang, W., Li, Z., Zhang, S., Yang, X., Zang, X., Wang, C., & Wang, Z. (2019). Triazine-based porous organic framework as adsorbent for solid-phase microextraction of some organochlorine pesticides. Journal of Chromatography A, 1602, 83–90. https://doi.org/10.1016/j.chroma.2019.06.001
Quan, C., Li, S., Tian, S., Xu, H., Lin, A., & Gu, L. (2004). Supercritical fluid extraction and clean-up of organochlorine pesticides in ginseng. The Journal of supercritical fluids, 31(2), 149–157. https://doi.org/10.1016/j.supflu.2003.11.003
Gonzalez-Curbelo, M. A., Socas-Rodriguez, B., & Herrera-Herrera, A. V., Gonzalez-Salamo, J., Hernandez-Borges, J., Rodriguez-Delgado, M. A. (2015). Evolution and applications of the QuEChERS method. Trac-Trends in Analytical Chemistry, 71, 169–185. https://doi.org/10.1016/j.trac.2015.04.012
Bruce-Vanderpuije, P., Megson, D., Ryu, S.H., Choi, G.H., Park, S.W., Kim, B.S., Kim, J.H., & Lee, H.S. (2021). A comparison of the effectiveness of QuEChERS, FaPEx and a modified QuEChERS method on the determination of organochlorine pesticides in ginseng. Plos One, 16(1). https://doi.org/10.1371/journal.pone.0246108
STB EN 15662-2017. Foods of plant origin. Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE-QuEChERS-method]. Minsk: BelGISS, 2017. 94 p. (in Russ.).
EURACHEM/CITAC Guide. Quantifying Uncertainty in Analytical Measurement.
Q2(R1) Validation of Analytical Procedures: Text and Methodology Guidance for Industry.
SANTE 11312/2021. Analytical quality control and method validation procedures for pesticide residues analysis in food and feed.
Copyright (c) 2022 Yekatsiaryna М. Pliashak, Alena I. Palianskikh, Ludmila L. Belysheva, and Alina I. Baturevich

This work is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.