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Natürel Sızma Zeytinyağlarında Bazı Pestisit Kalıntılarının GPC-GC Yöntemiyle Belirlenmesi

Yıl 2019, Sayı: 22, 11 - 18, 30.07.2019

Öz

Özet

Amaç: Bu çalışmada Bursa ve çevresinde üretilen
naturel sızma zeytinyağı örneklerinde bazı pestisit kalıntılarının Gel
Permeation Chromatography-Gas Chromatography yöntemiyle belirlenmesi ve mevcut
kalıntı durumunun ortaya konması amaçlanmıştır.

Materyal ve Yöntem: Bu amaçla Bursa ve çevresinde üretilen
36 adet naturel sızma zeytinyağı örneğinde azinphos-methyl, chlorpyrifos,
cyfluthrin, cypermethrin, deltamethrin, diazinon, dimethoate, endosülfan (alfa,
beta), fenitrothion, fenthion, formothion, lambda cyhalothrin, malathion,
methidathion, parathion methyl, monocrotophos, omethoate, phenthoate,
phosphamidone, tetradifon ve trichlorfon pestisit etken maddeleri analiz
edilmiştir.

Bulgular: Analizler DFG-S19 metodu kullanılarak
gerçekleştirilmiştir. Jel Geçirgenlik Kromatografisi (Gel Permeation
Chromatography, GPC) kullanılarak yağ molekülleri uzaklaştırıldıktan sonra
örnekler GC-ECD ve GC-FPD koşullarında analiz edilmiş ve GC-MS’ de doğrulama
yapılmıştır.









Sonuç: Yapılan çalışmalardaki geri
kazanım oranları %71,0-%118,9 aralığında bulunmuştur. Analiz edilen örneklerin
2 tanesinde hiçbir pestisit kalıntısı tespit edilmemiş iken diğer örneklerde yalnızca
chlorpyrifos kalıntısı tespit edilmiştir. Chlorpyrifos kalıntısı 5 örnekte
ölçüm limiti (Limit of Quantification, LOQ) olan 10 µg/kg’ın altında, 19
tanesinde 10-50 µg/kg aralığında, 10 tanesinde ise Türk Gıda Kodeksi
Pestisitlerin Maksimum Kalıntı Limitleri Yönetmeliği’nde sofralık zeytin ve
yağlık zeytin için belirtilen maksimum kalıntı limiti (Maximum Residue Limit, MRL)
değeri olan 50 µg/kg’dan daha yüksek bulunmuştur.
Abstract



Objective: In this study, performing residue
analyses of some pesticides in extra virgin olive oil, produced in Bursa region,
by applying Gel Permeation-Gas Chromatography method are aimed.



Materials and
Methods:
For this
purpose, residue analyses of azinphos methyl, chlorpyrifos, cyfluthrin,
cypermethrin, deltamethrin, diazinon, dimethoate, endosülfan (alfa, beta), fenitrothion,
fenthion, formothion, lambda cyhalothrin, malathion, methidathion, parathion
methyl, monocrotophos, omethoate, phenthoate, phosphamidone, tetradifon,
trichlorfon were performed according to DFG-S19 method in 36 extra virgin olive
oil samples.



Results: After removing lipid molecules by
Gel Permeation Chromatography (GPC) samples were analysed in GC-ECD and GC-FPD
conditions, then verification was made by GC-MS.



Conclusion: Recoveries of spiked extra virgin
olive oil samples ranged from 71,0% to 118,9%. No pesticide residues were determined
in two samples while only chlorpyrifos residue was determined in the rest of
samples. Residue level of chlorpyrifos in 5 samples was found below 10 µg/kg,
which is determined as LOQ, and between range of 10-50 µg/kg in 19 samples. In
10 samples chlorpyrifos residue level exceeded maximum residue limit (MRL) of
50 µg/kg defined in Turkish Food Codex for olives.

Kaynakça

  • Amvrazi, E.G. and Albanis, T.A., 2008. Multiclass Pesticide Determination in Olives and Their Processing Factors in Olive Oil: Comparison of Different Olive Oil Extraction Systems. J. Agric. Food Chem. 56: 5700–5709.
  • Amvrazi, E.G. and Albanis, T.A., 2009. Pesticide Residue Assessment in Different Types of Olive Oil and Preliminary Exposure Assessment of Greek Consumers to The Pesticide Residues Detected, Food Chemistry 113, 253–261.
  • Anagnostopoulos, C. and Miliadis, G.E., 2013. Development and Validation of an Easy Multiresidue Method for the Determination of Multiclass Pesticide Residues Using GC–MS/MS and LC–MS/MS in Olive Oil and Olives. Talanta112: 1–10.
  • Anonim, 1994. Gel-Permeation Cleanup. American Regulation USEPA SW-846 Method 3640A.
  • Anonim, 1999. Collection of Official Methods under Article 35 of the German Federal Act, DFG Method S19, L00.00.34-Modular Multiple Analytical Method for the Determination of Pesticide Residues in Foodstuffs (Extended and Revised Version of the DFG Method S 19).
  • Anonim, 2007. AOAC Official Method 2007.01 “Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate”.
  • Anonim, 2002. U.S. Environmental Protection Agency. 2002. Interim Reregistration Eligibility Decision for Chlorpyrifos. Washington, DC: U.S. EPA, Office of Prevention, Pesticides, and Toxic Substances. EPA 738-R-01-007. http://www.epa.gov/oppsrrd1/REDs/chlorpyrifos_ired.pdf.
  • Anonim, 2012. Scientific Report of EFSA. The 2012 European Union Report on Pesticide Residues in Food.
  • Anonim, 2014a. EFSA 2014. Conclusion on the Peer Review of the Pesticide Human Health Risk Assessment of the Active Substance Chlorpyrifos. EFSA Journal; 12(4):3640.
  • Anonim, 2014b. European Commission (EC) 2014. Commission Implementing Regulation (EC) No 400/2014 Of 22 April 2014 Concerning a Coordinated Multiannual Control Programme of the Union for 2015, 2016 and 2017 to Ensure Compliance with Maximum Residue Levels of Pesticides and to Assess the Consumer Exposure to Pesticide Residues in and on Food of Plant and Animal Origin. The Official Journal of the European Union, L119, 44–56.
  • Anonim, 2015. European Commission (EC) 2015. Commission Implementing Regulation (EU) 2015/ 595 of 15 April 2015 Concerning a Coordinated Multi Annual Control Programme of the Union for 2016, 2017 and 2018 to Ensure Compliance with Maximum Residue Levels of Pesticides and to Assess the Consumer Exposure to Pesticide Residues in and on food of Plant and Animal Origin. The Official Journal of the European Union, L99, 7–20. EU Reference Laboratories for R
  • Anonim, 2016. Manisa Ticaret Borsası. https://manisatb.org.tr/518/Haber/chlorpyrifos-ethyl-aktif-maddesi-ve-bu-aktif-maddeyi-iceren-bitki-koruma-urunleri-yasaklanmistir. Erişim tarihi: 15.02.2018.
  • Anonim, 2017. SANTE/11813/2017, Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticide Residues and Analysis in Food and Feed. European Commission Directorate General for Health and Food Safety.
  • Anonim, 2018a. EU Pesticides database. http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public. Erişim tarihi: 01.12.2018.
  • Anonim, 2018b. İşleme Faktörleri (İf) Veritabanı. www.tarimorman.gov.tr/Konu/1757/Pestisit_Kalinti_Limit_Degerlendirmesi_Isleme_Faktor. Erişim Tarihi: 15.03.2018.
  • Ballesteros, E., Sanchez, A.G. and Martos, N.R., 2006. Simultaneous Multidetermination of Residues of Pesticides and Polycyclic Aromatic Hydrocarbons in Olive and Olive-Pomace Oils by Gas Chromatography/Tandem Mass Spectrometry. Journal of Chromatography A, 1111: 89–96.
  • Beyer, A. and Biziuk, M., 2008. Applications of Sample Preparation Techniques in The Analysis of Pesticides and PCBs in Food. Food Chemistry, 108, 669-680. Durmaz, A. ve Tiryaki, O., 2018. Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, 4:2: 33-45.
  • Fernandez-Alba, A.R. and Garcia-Reyes, J.F., 2008. Large-Scale Multi-Residue Methods for Pesticides and Their Degradation Products in Food by Advanced LC-MS, Trends in Analytical Chemistry, 27, 973-990.
  • Garcia-Reyes, J.F., Ferrer, C., Gomez-Ramos, M.J., Molina-Diaz, A. and Fernandez-Alba, A.R., 2007. Determination of Pesticide Residues in Olive Oil and Olives, Trends in Analytical Chemistry, 26, 239-251.
  • Hakme, E., Lozano, A., Ferrer, C., Díaz-Galiano, F.J. and Fernandez-Alba, A.R., 2018. Analysis of Pesticide Residues in Olive Oil and Other Vegetable Oils. Trends in Analytical Chemistry 100: 167-179.
  • Kruve, A., Kunnapas, A., Herodes, K. and Leito, I., 2008. Matrix Effects in Pesticide Multi-Residue Analysis by Liquid Chromatography- Mass Spectrometry, J Chromatography A, 1187, 58-66.
  • López-Blanco, R., Moreno-González, D., Nortes-Méndez, R., García-Reyes, J.F., Molina-Díaz, A. And Gilbert-López, B., 2018. Experimental and Theoretical Determination of Pesticide Processing Factors to Model Their Behavior During Virgin Olive Oil Production. Food Chemistry 239: 9–16.
  • Sanchez, A.G., Martos, N.R. and Ballestero, E. 2005. Multiresidue Analysis of Pesticides in Olive Oil by Gel Permeation Chromatography Followed by Gas Chromatography–Tandem Mass-Spectrometric Determination, Analytica Chimica Acta, 558, 53–61.
  • Tiryaki, O. and Aysal, P., 2005. Applicability of TLC in Multiresidue Methods for the Determination of Pesticides in Wheat Grain, Bull. Environ. Contam. Toxicol., 75:1143–1149. DOI: 10.1007/s00128-005-0868-8.
Toplam 24 adet kaynakça vardır.

Ayrıntılar

Birincil Dil Türkçe
Bölüm Gıda ve Yem Bilimi-Teknolojisi Dergisi
Yazarlar

Sema Demir Bu kişi benim

Hakan Tosunoğlu Bu kişi benim 0000-0003-2163-657X

Altan Deniz Bu kişi benim 0000-0003-4358-5822

Yayımlanma Tarihi 30 Temmuz 2019
Yayımlandığı Sayı Yıl 2019 Sayı: 22

Kaynak Göster

APA Demir, S., Tosunoğlu, H., & Deniz, A. (2019). Natürel Sızma Zeytinyağlarında Bazı Pestisit Kalıntılarının GPC-GC Yöntemiyle Belirlenmesi. Gıda Ve Yem Bilimi Teknolojisi Dergisi(22), 11-18.

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Gıda ve Yem Bilimi-Teknolojisi Dergisi  CC BY-NC-ND 4.0 lisansı altında lisanslanmıştır
 Journal of Food and Feed Science-Technology is licensed under CC BY-NC-ND 4.0