Natürel Sızma Zeytinyağlarında Bazı Pestisit Kalıntılarının GPC-GC Yöntemiyle Belirlenmesi

ÖzetAmaç: 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.

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