A determination method of ethylene oxide (ETO) and 2-chloro-ethanol (2-CE) in foods, especially those with high-fat content, by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. The analysis was performed with a TG-WAX column (60 m × 0.32 mm × 1 µm), with a programmable temperature vaporization-large volume injection method (PTV-LVI). ETO, 2-CE, and isotope internal standard 2-chloroethanol-d4 (2-CE-d4) were extracted by the QuOil (a variation of QuEChERS method), in combination with the use of stainless-steel balls, especially effective with high-fat matrices and analyzed by gas chromatography-mass spectrometry (GC-MS/MS). For both compounds, the method has high specificity and selectivity with a detection limit of 0.003 mg/kg, the linear range of 0.01 - 0.2 mg/kg, reproducibility and recovery meet AOAC requirements. This method has been applied to analyze 1668 samples during the period 2021-2022 at the National Institute for Food Control (NIFC).
ethylene oxide, 2-chloro-ethanol, QuOil, stainless steel balls, GC-MS/MS.
[1]. Food Safety AUTHORITY OF IRELAND, “Recall of Certain Batches of Instant Noodle Products due to the Presence of the Unauthorised Pesticide Ethylene Oxide.” Aug. 20, 2021. [Online]. Available: https://www.fsai.ie/news_centre/food_alerts/instant_noodles_ethylene_oxide_recall.html [Accessed Aug. 08, 2022].
[2]. Cultivated plants, “Council Directive 91/414/EEC concerning the placing of plant protection products on the market.” 1991. [Online]. Available: https://www.ecolex.org/details/legislation/council-directive-91414eec-concerningthe-placing-of-plant-protection-products-on-the-market-lex-faoc018635/ [Accessed Aug. 08, 2022].
[3]. Centers for Disease Control and Prevention, “Ethylene Oxide | NIOSH | CDC,” Dec. 02, 2020. [Online]. Available: https://www.cdc.gov/niosh/topics/ethyleneoxide/default.html [Accessed Aug. 08, 2022].
[4]. A. S. de Oliveira et al., “Infographics and Pericyclic Reactions: Multimodal Resources in Teaching of Organic Chemistry,” Creative Education., vol. 07, no. 15, pp. 2163-2174, 2016.
[5]. “Ethylene Oxide - IARC Monographs on the Evaluation of Carcinogenic Risks to Humans. Lyon: International Agency for Research on Cancer. 2008. pp. 185–287. ISBN 978-92-832-1297-3. Archived from the original on 25 December 2016. Retrieved 11 January 2019.” Jan. 16, 2017. [Online]. Available: https://web.archive.org/web/20170116233424/http://monographs.iarc.fr/ENG/Monographs/vol97/mono97-7.pdf [Accessed: Sep. 07, 2021].
[6]. “EUR-Lex - 32015R0868 - EN - EUR-Lex.” Jun. 10, 2015. [Online]. Available: https://eur-lex.europa.eu/legal-content/EN/TXT/?uri=CELEX%3A32015R0868 [Accessed Aug. 09, 2022].
[7]. National Archives, “40 CFR 180.151 -- Ethylene oxide; tolerances for residues.” Sept. 11, 2009. [Online]. Available: https://www.ecfr.gov/current/title-40/chapterI/subchapter- E/part-180/subpart-C/section-180.151 [Accessed Sep. 05, 2022].
[8]. H. Canada, “Proposed Maximum Residue Limit PMRL2019-29, Ethylene Oxide,” Jan. 02, 2020. [Online]. Available: https://www.canada.ca/en/health-canada/services/consumer-product-safety/pesticides-pest-management/public/consultations/proposed-maximum-residue-limit/2019/ethylene-oxide/document.html [Accessed Sep. 05, 2022].
[9]. The Japan Food Chemical Research Foundation, "The Japanese Positive List System for Agricultural Chemical Residues in Foods" [Online]. Available: https://www.ffcr.or.jp/en/zanryu/the-japanese-positive/the-japanese-positive-listsystem-for-agricultural-chemical-residues-in-foods-enforcement-on-may-29-.html [Accessed Sep. 05, 2022].
[10]. The Australia New Zealand Food Authority, "Application A445 - Maximum Residue Limits – Section 37.” Mar. 13, 2000. [Online]. Available: https://www.foodstandards.gov.au/code/applications/documents/A445_FARs37.pdf [Accessed: Sep. 05, 2022].
[11]. European Commission, “Summary of the Technical Meeting on Ethylene Oxide (ETO).” Jan. 20, 2022 [Online]. Available: https://food.ec.europa.eu/system/files/2022-02/rasff_ethylene-oxide-incident_e410_crisis-coord_20220120_sum.pdf [Accessed: Aug. 31, 2022].
[12]. EN 15662:2018, “Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method”
[13]. CEN/TS 17062:2019, “Foods of plant origin - Multimethod for the determination of pesticide residues in vegetable oils by LC-MS/MS (QuOil).”
[14]. K. G. Jensen, “Determination of ethylene oxide residues in processed food products by gas-liquid chromatography after derivatization,” Z. Fr Lebensm.-Unters. -Forsch., vol. 187, no. 6, pp. 535-540, 1998.
[15]. P. Aitkenhead and A. Vidnes, “Simple and Accurate Method for Determination of Ethylene Chlorohydrin in Dried Spices and Condiments,” Journal of AOAC International, vol. 71, no. 4, pp. 729-731, 1988.
[16]. F. Tateo and M. Bononi, “Determination of ethylene chlorohydrin as marker of spices fumigation with ethylene oxide,” Journal of Food Composition and Analysis, vol. 19, no. 1, pp. 83-87, 2006.
[17]. AOAC Official Methods of Analysis (2012), "Appendix F: Guidelines for standard method performance requirements" [Online]. Available: http://www.eoma.aoac.org/app_f.pdf [Accessed: Nov. 22, 2021].
[18]. EU Reference Laboratories for Residues of Pesticides - Single Residue Methods, “Analysis of Ethylene Oxide and its Metabolite 2-Chloroethanol by the QuOil or the QuEChERS Method and GC-MS/MS.” Dec. 2020. [Online]. Available: https://www.eurl-pesticides.eu/library/docs/srm/EurlSrm_Observation_EO_V1.pdf [Accessed: Aug. 08, 2022]
[19]. Agilent Technoligies, “Ethylene Oxide & 2-Chloroethanol analysis in Foods using Triple Quadrupole GC/MS/MS: Consumables Workflow Ordering Guide,” pp. 7.
[20]. P. O. of the E. Union, “Commission Implementing Regulation (EU) 2021/808 of 22 March 2021 on the performance of analyti cal methods for residues of pharmacologically active substances used in food-producing animals and on the interpretation of results as well as on the methods to be used for sampling and repealing Decisions 2002/657/EC and 98/179/EC (Text with EEA relevance), C/2021/1772,” Mar. 22, 2021. [Online]. Available: http://op.europa.eu/en/publication-detail/-/publication/3dc2b06b-b9cf-11eb-8aca-01aa75ed71a1/language-en [Accessed Sep. 06, 2022].
[21]. Codex Alimentarius, “Guidelines on estimation of uncertainty of results,” pp. 9.
[22]. “ISO/TS 21748:2004 Guidance for the use of repeatability, reproducibility and trueness estimates in measurement uncertainty estimation" [Online]. Available: https://www.iso.org/cms/render/live/en/sites/isoorg/contents/data/standard/03/46/34686.html [Accessed Nov. 25, 2021].
[23]. CVUA Stuttgart, "Chemicals Rather than Bacteria? – Neither is Permitted in the EU” Dec. 10, 2020. [Online]. Available: https://www.ua-bw.de/pesticides/beitrag_en.asp?subid=1&ID=3295&lang=EN [Accessed Sep. 06, 2021].