Polisilik aromatik hidrokarbon (PAH)' lardan benzo (A) pirenin sızma, riviera ve prina zeytinyağlarında belirlenmesi

Bu çalışma, 20 adet naturel sızma zeytinyağı, 20 adet riviera zeytinyağı ve 10 adet rafine prina yağında bulunan benzo(a)piren (BaP) miktarlarını belirlemek amacıyla yapılmıştır. Örneklerin hazırlanmasında silika kartuş kullanılmış ve katı faz ekstraksiyonu yapılmıştır. Analizler fluoresans dedektörü ile kombine edilmiş HPLC cihazında yapılmıştır. Yöntemde ortalama geri alma oranı % 76,08 ± 1,49, tespit edilebilir en düşük miktar 0,3 µg/kg olarak belirlenmiştir. Bu bilgiler, yöntemin zeytinyağlarındaki BaP miktarının belirlenmesinde rutin olarak kullanılabileceğini göstermiştir. Analizi yapılan naturel sızma zeytinyağı örneklerinin 3'ünde 0,330 µg/kg ile 0,870 µg/kg arasında BaP tespit edilmiştir. Bu örnekler için ortalama BaP miktarı 0,539 ± 0,167µg/kg'dır. Riviera zeytinyağının 8'inde tespit edilebilir düzeyde BaP kalıntısına rastlanmazken, 12'sinde 2,465 µg/kg seviyesine kadar BaP bulunmuştur. BaP tespit edilen örneklerde ortalama miktar 0,737 ± 0,192 µg/kg olarak saptanmıştır. Prina yağlarının çoğunda yüksek miktarlarda BaP bulunmuştur. BaP tespit edilen 7 örnekte ortalama miktar 31,472 ± 7,42 µg/kg (en az: 0,460 µg/kg, en çok: 58,241 µg/kg)'dır. Naturel sızma zeytinyağı, riviera zeytinyağı ve prina yağlarının ortalamaları arasındaki farklılıkların irdelenmesinde varyans analizi tekniği kullanılmış ve ortalamalar arasındaki farkların önemli olduğu saptanmıştır. Farklı yağ gruplarının tespitinde ise DUNCAN testinden yararlanılmış, sadece prina yağı ortalaması ile diğer yağ örneklerinin ortalamaları arasındaki farkların istatistik olarak önemli olduğu belirlenmiştir (p< 0,01).

Determination of benzo (A)pyrene from polycyclic aromatic hydrocarbons in extra virgin, riviera and olive pomace oils

This study was carried out to determine the amount of benzo(a)pyrene in 20 of extra virgin olive oils, 20 of riviera olive oils and 10 of refined olive pomace oils. Solid phase extraction (silica cartidge) was used in the preparation of samples. Analyses were made by HPLC combined with fluorescence detector. In this method, mean of recovery was found % 76.08 ± 1.49 and limit of detection was 0.3 µg/kg. The findings showed that this method can be used for determining benzo(a)pyrene in olive oils for routine analysis. In three of the extra virgin olive oil samples analysed, BaP was determined between 0.330 µg/kg and 0.870 µg/kg and mean concentration was 0.539 ± 0.167µg/kg. BaP was not determined at limit of dedection in eight of riviera olive oils samples whereas; it was found 2.465 µg/kg in 12 of these samples. In the samples containing BaP, mean concentration of BaP was determined 0.737 ± 0.192 µg/kg. In the most of the olive pomace oils, BaP was found at the highest level. The mean concentration of BaP was 31.472 ± 7.42 µg/kg (min: 0.460 µg/kg, max: 58.241 µg/kg) in 7 samples containing BaP. Results were analyzed by the one-way analysis of variance for determining the differences among the BaP concentrations of extra virgin olive oils, riviera olive oils, olive pomace oils. It was found that the mean concentrations were significantly different (p≤0.09) DUNCAN test for comparision among means, only mean concentration of BaP in olive pomace oil was statistically significant (p< 0.01).

___

  • 1.Tuominen J. 1990. Determination of polycyclic aromatic hydrocarbons by gas chromatography/mass spectrometry and method development in supercritical fluid chromatography. Technical Research Centre of Finland, Publications 60 Espoo, Finland
  • 2.Williams PT. 1990. Sampling and analysis of polycyclic aromatic compounds from Combustion systems. Journal of The Institue of Energy, 63; 22
  • 3.Moret S, Conte L. S. 2000. Polycyclic aromatic hydrocarbons in edible fats and oils: occurrence and analytical methods. Journal of Chromatography A, 882; 245-253
  • 4.Kaya S., Pirinçci, i., Bilgili A. 1998. Veteriner Hekimliğinde Toksikoloji. Medisan Yayın Serisi:35,1. Baskı, 452 s, Ankara.
  • 5.Moret, S, Conte L. S. 2002.A rapid method for polycyclic aromatic hydrocarbon determination in vegetable oils. Journal of Separation Science, 25; 96-100.
  • 6.Anonim. 2003b. Refik Saydam Hıfzısıhha Merkezi Başkanlığı Çevre Sağlığı Araştırma Müdürlüğü Hava Kirliliğine Genel Bakış. 47-60 s.
  • 7.Anonim. 1983. International Agency for Research on Cancer (İARC). Monographs on the evaluation of carcinogenic risk of chemical to humans, polynuclear aromatic compounds. Part 1, France.
  • 8.Dıraman E. 1994. Aspirin ve antioksidantlarin (butylated hydroxyanisole ve askorbik asit) farelerde (mus musculus) benzo(a)pyrene hidroksilaz aktivitesi üzerine etkileri. Ondokuz Mayıs Üniversitesi Fen Bilimleri Enstitüsü, Doktora Tezi, Samsun.
  • 9.Shuguang L, Dinhua, P, Guoxiong, W. 1994. Analysis of polycyclic aromatic hydrocarbons in cooking oil fumes. Archives of Environmental Health, 49(2); 119-122.
  • 10.Moret S, Piani B, Bortolomeazzİ R, Conte L S. 1997. HPLC determination of polycyclic aromatic hydrocarbons in olive oils. Z. Lebensm Unters Forsch A, 205; 116-120.
  • 11.Pupin, A. M., Toledo, M. C. F.1996. Benzo(a)pyrene in olive oils on the Brazilian market. Food Chemistry, 55(2); 185-188.
  • 12.Troche, V. S, Falcon, G. M. S, Amigo, G. S, Yusty, L. M. A, Lozano, S. J. 2000. Enrichment of benzo(a)pyrene in vegetable oils and determination by HPLC-FL. Talanta, 51; 1069-1076
  • 13.Gfrerer, M, Lankmayr, E. 2003. Microwave-assisted saponification for the determination of 16 polycyclic aromatic hydrocarbons from pumpkin seed oils. Journal of Separation Science, 26; 1230-1236.
  • 14.Stijn, F. V, Kerkhoff, M. A. T, Vandeginste, B. G. M 1996. Determination of polycyclic aromatic hydrocarbons in edible oils and fats by on-line donor-acceptor complex chromatography and high-performance liquid chromatography with fluorescence dedection. Journal Chromatography A, 750; 263-273.
  • 15.Moreda, W, Perez-Camino, M. C, Cert, A. 2001. Gas and liquid chromatography of hydrocarbons in edible vegetable oils. Journal of Chromatography A, 936; 159-171.
  • 16.Anonim. 2001a. Contaminants- Polycyclic aromatic hydrocarbons in olive residue oil.
  • 17.Anonim.2002a. European Commission. Directorate F- Food and Veterinary Office.Final report of a mission carried out in France from 21st to 30th october 2002 in order to assess the control measures in place for vegetable oil production . and in particular for the assessment of controls on PAH (polycyclic aromatic hydrocarbons) contamination of such oils.
  • 18.Anonim. 2003a. Prinanın bir yakıt olarak kullanımı ve eldesi. Gazi Üniv.
  • 19.Bogusz, M. J, Hajj, S. A. E, Ehaideb, Z„ Hassan, H, Al-Tufail, M. 2004. Rapid determination of benzo(a)pyrene in olive oils samples with solid-phase extraction and low-pressure, wide-bore gas chromatography-mass spectrometry and fast liquid chromatography with fluorescence detection. Journal of Chromatography A, 1026; 1-7.
  • 20.Larsson, B. K, Erikson, A. T, Cervenka, M. 1987. Polycyclic aromatic hydrocarbons in crude and deodorized vegetable oils. JAOCS, 64(3);365-370.
  • 21.Moret, S, Dudine, A., Conte, L. S. 2000. Processing effects on the polyaromatic hydrocarbon content of grapeseed oil. JAOCS, 77(12); 1289-1292.
  • 22.Cert, A., Moreda, W., Perez-Camino, M. C. 2000. Chromatographic analysis of minor constituents in vegetable oils. Journal of Chromatography A, 881; 131-148.
  • 23.Perrin, J. L, Poirot, N. Liska, P., Thienpont, A., Felix, G. 1993. Trace enrichment and HPLC analysis of PAHs in edible oils and (at products, using liquid chromatography on electron acceptor stationary phases in connection with reverse phase and fluorescence detection. Fat Sci Technol., 95; 46-51.
  • 24.Anonim 2003c. Removal of PAH from vegetable oil.
  • 25.Anonim 2003d. Polynuclear aromatic hydrocarbons removal.
  • 26.Bogan, B. W., Trbovic, V., Paterek, J. R. 2003. Inclusion of vegetable oils in Fenton's chemistry for remediation of PAH-contaminated soils. Chemosphere, 50; 15-21.
  • 27.Osborne, M. R., Crosby, N. T. 1987. Benzopyrenes. Cambridge University Press, 128-129, UK.
  • 28.Anonim 2004a. Outline of the amendment of the cabinet ordinance and the ministerial ordinance for the Jaw for the control of house hold products containing harmful substances.
  • 29.Speer, K., Steeg, E., Horstmann, P., Kühn, T., Montag,A.1990.Determination and distribution of polycyclic aromatic hydrocarbons in native vegetable oils, smoked fish products, mussels and oysters and bream from the River Elbe. Journal of High Resolution Chromatography, Vol 13 (February);104-111.
  • 30.BjÖrseth, A., Becher, G. 1986. PAH in work atmospheres: occurrence and determination. Boca Raton, Fİ: CRC Pres; 103-116
  • 31.Barranco, A. Alonso-Salces, R. M., Bakkali, A., Berrueta, L. A., Gallo, B., Vicente, F., Sarobe, M. 2003a. Solid-phase clean-up in the liquid chromatographic determination of polycyclic aromatic hydrocarbons in edible oils. Journal of Chromatography A, 988; 33-40.
  • 32.Anonim 2002b. Polyaromatic hydrocarbons (PAH) in evening primrose oil,
  • 33.Anonim 2002d. Türk gıda kodeksi gıda maddelerinde belirli bulaşanların maksimum seviyelerinin belirlenmesi hakkında tebliğ (tebliğ no: 2002/63). Resmi gazete: 23 Eylül 2002 tarihli ve 24885 sayılı tebliğ.
  • 34.Moret, S., Cericco, V., Conte, L. S. 2001. On-line solvent evaporator for coupled normal phase-reversed phase high-performance liquid chromatography systems: Heavy polycyclic aromatic hydrocarbons analysis. J. Microcolumn Separations, 13(1); 13-18.
  • 35.Camacho, M. L., Alcaide, I. V., Mendez, M. V. R. 2003. Elimination of polycyclic aromatic hydrocarbons by bleaching of olive pomace oil. Eur. J. Lipid Sci. Technol., 105; 9-16.
  • 36.Pollard, S.J.T., Sollars, C.J., Perry, R. 1993. The reuse of spent bleaching earth: a feasibility study in waste minimisation for the edible oil industry. Bioresource technology, 45; 53-58.
  • 37.Anonim 1993. Guidelines on good laboratory practice in pesticide residue analysis. Food and Agricultural Organization of United Nations. World Health Organization, Rome.
  • 38.Anonim 2004c.Food Standarts Agency.Update on EU discussions on chemical contaminants. Annex II. Sample preparation and criteria for methods of analysis used in official checking of the levels of benzo(a)pyrene in foods.