İncirlerde insektisit kalıntılarının araştırılması ve sağlık risk değerlendirmesi

Öz

Bu çalışma 2022 yılında Aydın ilinde yoğun incir, Ficus carica L. (Rosales: Moraceae) üretiminin yapıldığı lokasyonlardan alınan 92 yaş ve 50 kuru incir numunesinde insektisit, akarisit ve nematisit kalıntılarının tespiti için gerçekleştirilmiştir. Analiz metodu SANTE 11312/2021’e göre doğrulanmıştır. Ortalama geri kazanımlar %73,2 ile %119,6 arasında olup yöntemin tekrarlanabilirliği (RSDr) ve laboratuvar içi tekrar üretilebilirliği (RSDwR) için ≤ %20 ve genişletilmiş ölçüm belirsizlikleri %50'nin altındadır. Bu veriler tatmin edici analitik performansı göstermektedir. Toplamda 114 farklı insektisitin tarandığı çalışmada, 92 yaş incir numunesinin 13’ünde bifenazate, 3’ünde etoxazole, 5’inde spiromesifen, 6’sında ise hem bifenazate hem spiromesifen olmak üzere toplam 27 numunede pestisit kalıntısı kaydedilmiştir. Kuru incir örneklerinde tespit edilebilir kalıntıya rastlanmamıştır. Bifenazate tespit edilen örneklerin tamamı Avrupa Birliği Maksimum Kalıntı Limitlerinin (AB-MRL) üzerindedir. Etoxazole ve spiromesifen etken maddeleri incirde ruhsatsız olup, numunelerde tespit edilen etoxazole kalıntıları AB-MRL üzeri, spiromesifen ise AB-MRL altıdır. Tespit edilen insektisitlerin akut ve kronik sağlık risk indeksi 1'den düşük bulunmuştur. Risk değerlendirmesi incir tüketiminin tüketiciler için güvenli olduğunu göstermiştir.

Anahtar Kelimeler

• Kuru incir
• incir
• LC-MS/MS
• pestisit kalıntısı
• QuEChERS

Investigation of insecticide residues in fig and health risk assessment

Abstract

This study aimed to detect insecticide, acaricide, and nematicide residues in 92 fresh and 50 dried fig samples collected from locations with intensive fig, Ficus carica L. (Rosales: Moraceae) production in Aydın, Türkiye in 2022. The analysis method was validated according to SANTE 11312/2021 guidelines. The recoveries ranged between 70% and 120%, with repeatability (RSDr) and within-laboratory reproducibility (RSDwR) ≤ 20% and expanded measurement uncertainties below 50% for all insecticides indicating satisfactory analytical performance. In total, 114 different insecticides were screened, revealing residues in 27 samples. Bifenazate was detected in 13 samples, etoxazole in 3 samples, spiromesifen in 5 samples, and both bifenazate and spiromesifen in 6 samples. No detectable residues were found in the dried fig samples. All samples in which bifenazate was detected were above the European Union Maximum Residue Limits (EU-MRL). Etoxazole and spiromesifen, unauthorized in figs, showed etoxazole residues above EU-MRLs, while spiromesifen residues were below EU-MRLs. The acute and chronic health risk indices for the insecticides were found to be below 1, indicating low health risks associated with fig consumption. The risk assessment suggests that fig consumption is safe for consumers.

Keywords

• Dried fig
• fig
• LC-MS/MS
• pesticide residue
• QuEChERS

Kaynakça

1. Akoto, O., S. Gavor, M. K. Appah & J. Apau, 2015. Estimation of human health risk associated with the consumption of pesticide-contaminated vegetables from Kumasi Ghana. Environmental Monitoring and Assessment, 187 (5): 1-9.
2. Akşit, T., F. Özsemerci & İ. Çakmak, 2003. Aydın ilinde incir ağaçlarında saptanan zararlı türler. Turkish Journal of Entomology, 27 (3): 181-189 (in Turkish with abstract in English).
3. Anonymous, 2023. Türk gıda kodeksi pestisitlerin maksimum kalıntı limitleri yönetmeliği. (Web page: https://www.resmigazete.gov.tr/eskiler/2021/09/20210927M1-1.htm) (Date accessed: November 2023) (in Turkish).
4. Anonymous, 2024. Plant Protection Products Database. (Web page: https://bku.tarimorman.gov.tr/Arama/Index?csrt=11430343323884281979) (Date accessed: September 2024) (in Turkish).
5. AOAC, 2007. AOAC Official Method: Pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry. First Action 2007. (Web page: https://nucleus.iaea.org/sites/fcris/Shared%20Documents/SOP/AOAC_2007_01.pdf) (Date accessed: September 2024).
6. Aydin, S. & M. Ulvi, 2019. Residue levels of pesticides in nuts and risk assessment for consumers. Quality Assurance and Safety of Crops & Foods, 11 (6): 539-548.
7. Balkan T. & Ö. Yılmaz, 2022a. Investigation of insecticide residues in potato grown in Türkiye by LC-MS/MS and GC-MS and health risk assessment. Turkish Journal of Entomology, 46 (4): 481-500.
8. Balkan T. & Ö. Yılmaz, 2022b. Method validation, residue and risk assessment of 260 pesticides in some leafy vegetables using liquid chromatography coupled to tandem mass spectrometry. Food Chemistry, 384 (2022): 132516 (1-21).

9. Balkan, T. & K. Kara, 2022. Determination of pesticide residues and risk assessment in some vegetables grown in Tokat province. Plant Protection Bulletin, 62 (2): 26-35.
10. Çatak, H. & O. Tiryaki, 2020. Insecticide residue analyses in cucumbers sampled from Çanakkale open markets. Turkish Journal of Entomology, 44 (4): 449-460.
11. EC, 2002. European Commission: Commission Directive 2002/63/EC of 11 July 2002 establishing Community methods of sampling for the official control of pesticide residues in and on products of plant and animal origin and repealing Directive 79/700/EEC. Official Journal of the European Communities, L 187 (45): 30-43.
12. EC, 2005. European Commission: Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC Text with EEA relevance. Official Journal of the European Communities, L 70 (48): 1-16.
13. EFSA, 2015. European Food Safety Authority: Revisiting the International Estimate of Short-Term Intake (IESTI equations) used to estimate the acute exposure to pesticide residues via food. EFSA Supporting Publication, 12 (12): 1-81.
14. EU-MRL, 2022. European Union (EU-MRL) Pesticides Database: Pesticide Residues MRLs. Directorate General for Health & Consumers. (Web page: https://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/mrls/?event=search.pr) (Date accessed: November 2022).
15. EURACHEM, 2014. Eurachem Guide: The Fitness for Purpose of Analytical Methods – A Laboratory Guide to Method Validation and Related Topics, (2nd Ed. 2014). ISBN 978-91-87461-59-0. (Web page: https://www.eurachem.org/images/stories/Guides/pdf/MV_guide_2nd_ed_EN.pdf) (Date accessed: December 2022).
16. FAO, 2021. FAOSTAT, Crops and livestock products. (Web page: https://www.fao.org/faostat/en/#data/QCL) (Date accessed: September 2024).
17. Hasdemir, M., 2022. Agricultural Products Market, Fig. (Web page: https://arastirma.tarimorman.gov.tr/tepge/Belgeler/PDF%20Tar%C4%B1m%20%C3%9Cr%C3%BCnleri%20Piyasalar%C4%B1/2023-Temmuz%20Tar%C4%B1m%20%C3%9Cr%C3%BCnleri%20Raporu/%C4%B0NC%C4%B0R%20T%C3%9CP%20HAZ%C4%B0RAN%202023-TEPGE.pdf) (Date accessed: November 2023).
18. IUPAC, 2024. The PPDB-Pesticide properties database, international union of pure and applied chemistry. (Web page: http://sitem.herts.ac.uk/aeru/iupac/index.htm) (Date accessed: September 2024).
19. Liu, Y., D. Shen, S. Li, Z. Ni, M. Ding, C. Ye & F. Tang, 2016. Residue levels and risk assessment of pesticides in nuts of China. Chemosphere, 144 (2016): 645-651.
20. RASFF, 2024. Rapid Alert System for Food and Feed. (Web page: https://food.ec.europa.eu/safety/rasff-food-and-feed-safety-alerts_en) (Date accessed: September 2024).
21. Rosas-Sánchez, J., H. Saldarriaga-Noreña, L. A. Chávez-Almazán, M. A. Murillo-Tovar, I. I. Ramírez-Bustos, V. A. Leon-Hernández & E. Fernández-Herrera, 2023. Occurrence of pesticide residues in fig crops (Ficus carica L.), in Morelos, Mexico. Revista Internacional de Contaminación Ambiental, 39 (2023): 215-227.
22. SANTE, 2021. SANTE/11312/2021, Analytical quality control and method validation procedures for pesticide residues analysis in food and feed, 1-55. (Web page: https://food.ec.europa.eu/system/files/2022-02/pesticides_mrl_guidelines_wrkdoc_2021-11312.pdf) (Date accessed: September 2022).
23. Serbes, E. B. & O. Tiryaki, 2023. Determination of insecticide residues in “Bayramiç Beyazı” nectarines and their risk analysis for consumers. Turkish Journal of Entomology, 47 (1): 73-85.
24. Soydan, K. D., N. Turgut, M. Yalçın, C. Turgut & P. B. K. Karakuş, 2021. Evaluation of pesticide residues in fruits and vegetables from the Aegean region of Turkey and assessment of risk to consumers. Environmental Science and Pollution Research, 28 (22): 27511-27519.
25. Tatlı, Ö., 2006. Ege Bölgesine Özgü Bazı Yaş Meyve, Sebze ve Kurutulmuş Gıda Ürünlerinde Pestisit Kalıntı Düzeylerinin Tespiti. Çukurova Üniversitesi Fen Bilimleri Enstitüsü, Toprak Anabilim Dalı, (Unpublished) Yüksek Lisans Tezi, Adana, 120 s (in Turkish with abstract in English).
26. TGK-MRL, 2022. Republic of Turkey, ministry of food, agriculture and livestock, general directorate of food and control, department of plant protection products, MRL rates. (Web page: https://bku.tarimorman.gov.tr/MRLOrani/Index?csrt=2789820862056200932) (Date accessed: November 2022).
27. TUIK, 2022. Turkish Statistical Institute. Poultry production statistics. (Web page: https://biruni.tuik.gov.tr/medas/?kn=80&locale=en) (Date accessed: November 2022).
28. TUIK, 2023. Turkey Health Interview Survey. (Web page: https://data.tuik.gov.tr/Bulten/DownloadIstatistikselTablo?p=WEBW229PP/91tMV2m71fU6pRWq2F1ZD/lzOFFk0bNDi2rjAC8QDCRN62nr2M3n1K) (Date accessed: November 2023).