Phương pháp sắc ký khí khối phổ hai lần (GC-MS/MS) đã được nghiên cứu và thẩm định nhằm xác định ethylene oxide (ETO) và 2-chloro-ethanol (2-CE) trong thực phẩm, đặc biệt là những thực phẩm có hàm lượng chất béo cao. Phương pháp tách được thực hiện qua cột TG-WAX (60 m × 0,32 mm × 1 µm), với kỹ thuật tiêm thể tích lớn và hóa hơi với chương trình nhiệt độ (PTV-LVI). ETO, 2-CE, và nội chuẩn đồng vị 2-chloro-ethanol-d4 (2-CE-d4) được xử lý bằng phương pháp QuOil (một biến thể của phương pháp QuEChERS), kết hợp với việc sử dụng bi thép không gỉ, đặc biệt hiệu quả với chất nền có hàm lượng chất béo cao và được phân tích bằng phương pháp sắc ký khí khối phổ (GC-MS/MS). Phương pháp này có độ đặc hiệu và độ chọn lọc cao với giới hạn phát hiện 0,003 mg/kg, khoảng tuyến tính 0,01 - 0,2 mg/kg, độ tái lập và độ thu hồi đáp ứng các yêu cầu của AOAC. Phương pháp này đã được áp dụng để phân tích 1668 mẫu thực phẩm trong giai đoạn 2021-2022 tại Viện Kiểm nghiệm an toàn vệ sinh thực phẩm Quốc gia (NIFC).
ethylene oxide, 2-chloro-ethanol, QuOil, bi thép không gỉ, 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].