Cemil KÜREKÇİ, Sait TAN, Ali ARSLAN, Sara Betül ÖZGEN, Fatih SAKİN

PEYNİR NUMUNELERİNDE BİSFENOL A İÇİN KATI FAZ EKSTRAKSİYON METOTLARININ KARŞILAŞTIRILMASI

Bu çalışmada, dört farklı katı-faz ekstraksiyon metotunun peynir numunelerinden bisfenol A (BPA) ekstraksiyon performansı HPLC-FD kullanılarak kıyaslanmıştır. Metot validasyonları doğrusallık, geri kazanım, kesinlik, metodun belirlenme ve tayin alt sınırları (LOD/LOQ), bağıl standart belirsizlik parametreleri ile yapılmıştır. Buna ilaveten Elazığ ilinde satışa sunulan yirmi adet peynir numunesinde BPA miktarı belirlenmiştir. Bütün metotlar BPA’nın kantitatif analizi için düşük LOD (0.16-0.39 µg/kg) ve LOQ (0.53-1.30 µg/ kg) seviyelerinde iyi performans göstermişlerdir. Geri kazanım seviyeleri iki farklı ekleme miktarı (3-30 µg/kg) için ortalama %93.1 ve %100.8 aralığında hesaplanmıştır. Peynir numunelerinin %55’inde 0.75 µg/kg ve 8.46 µg/kg miktarları arasında BPA varlığı bulunmuştur ve günlük alım tahmini (EDI) 0,001 µg/kg vücut ağırlığı/gün olarak hesaplanmıştır. EDI sonuçlarına göre, peynir tüketimi tek başına BPA için önemli halk sağlığı riski ortaya çıkartmadığı, fakat sonuçlar süt ve süt ürünlerinde BPA’nın düzenli takibinin yapılması gerektiğini göstermiştir.

Anahtar Kelimeler:

Katı-faz ekstraksiyonu, Bisfenol A, PEYNİR, HPLC

A COMPARISON OF SOLID-PHASE EXTRACTION METHODS FOR BISPHENOL A IN CHEESE SAMPLES

In this study, four different solid phase extraction (SPE) methods were compared for the determination of bisphenol A (BPA) in cheese samples using HPLC-FD. All methods were validated according to the parameters; linearity, recovery, precision, detection and quantification limits (LOD-LOQ). Subsequently, BPA levels were determined in twenty cheese samples commercially available in Elazığ province. All the extraction methods showed good performances for quantitative analysis of PBA, achieving very low LOD (0.16-0.39 µg/kg) and LOQ (0.53-1.30 µg/ kg) values. The average fortification recoveries for spiked BPA (3-30 µg/kg) ranged between 93.1 and 100.8%. 55% of cheese samples had BPA concentration ranging from 0.75 µg/kg to 8.46 µg/kg and estimated daily intake (EDI) was measured as 0,001 µg/kg BW per day. On the basis of EDI, the consumption of cheese itself cannot be considered as significant health problem, but results impose a systematic monitoring of dairy products.

Keywords:

Solid-phase extraction, Bisphenol A, CHEESE, HPLC,

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Alnaimat AS, Barciela-Alonso MC, Bermejo-Barrera P. (2019). Determination of bisphenol A in tea samples by solid phase extraction andliquid chromatography coupled to mass spectrometry. Microchem J, 147, 598-604.
Andrade-Eiroa A, Canle M, Leroy-Cancellieri V, Cerdà V. (2016). Solid-phase extraction of organic compounds: A critical review (Part I). Trends Analyt Chem, 80: 641-654.
Azzouz A, Kailasa SK, Lee SS, Rascón AJ, Ballesteros E, Zhang M, Kim K-H. (2018). Review of nanomaterials as sorbents in solid-phase extraction for environmental samples. Trends Analyt Chem, 108: 347-369.
Ballesteros-Gómez A, Soledad R, Dolores PB. (2009). Analytical methods for the determination of bisphenol A in food. J Chromatogr A 1216: 449-469.
Bemrah N, Jean J, Rivière G, Sanaa M, Leconte S, Bachelot M., Deceuninck Y, Le Bizec B, Dauchy X, Roudot A-C, Camel V, Grob K, Feidt C, Picard-Hagen N, Badot P-M, Foures F, Leblanc J-C. (2014). Assessment of dietary exposure to bisphenol A in the French population with a special focus on risk characterization for pregnant French women. Food Chem Toxicol, 72: 90–97.
Cao XL, Perez-Locas C, Dufresne G, Clement G, Popovic S, Beraldin F, Dabeka RW, Feeley M. (2011). Concentrations of bisphenol A in the composite food samples from the 2008 Canadian total diet study in Quebec City and dietary intake estimates. Food Addit Contam, 28: 791–798.
Cunha S, Cunha C, Ferreira A, Fernandes J. (2012). Determination of bisphenol A and bisphenol B in canned seafood combining QuEChERS extraction with dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry. Anal Bioanal Chem, 404: 2453-2463.
EFSA (2015). Scientific Opinion on the risks to public health related to the presence of bisphenol A (BPA) in foodstuffs: executive summary. EFSA J, 13: 3978.
European Commission 2002/657/EC. (2002). Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results, Off J Eur Commun, L221: 8 – 36.
European Commission. (1996). European workshop on the impact of endocrine disruptors on human health and wildlife. Report of Proceedings from a Workshop held in Weybridge, UK, December 2-4, 1996. Report reference EUR 17549, European Commission, DG XII, Brussels, Belgium.
Geens T, Aerts D, Berthot C, Bourguignon JP, Goeyens L, Lecomte P, Maghuin-Rogister G, Pironnet A-M, Pussemier L, Scippo M-L, Van Loco J, Covaci A. (2012). A review of dietary and non-dietary exposure to bisphenol-A. Food Chem Toxicol, 50: 3725-3740.
Giulivo M, de Alda ML, Capri E, Barceló D. (2016). Human exposure to endocrine disrupting compounds: Their role in reproductive systems, metabolic syndrome and breast cancer. A review. Environ Res 151, 251-264.
Grumetto L, Gennari O, Montesano D, Ferracane R, Ritieni A, Albrizio S, Barbato F. (2013). Determination of five bisphenols in commercial milk samples by liquid chromatography coupled to fluorescence detection. J Food Protect, 76: 1590–1596.
Grumetto L, Montesano D, Seccia S, Albrizio S, Barbato F. (2008). Determination of bisphenol A and bisphenol B residues in canned peeled tomatoes by reversed-phase liquid chromatography. J Agric Food Chem, 56, 10633-10637.
Hayaloğlu AA, Özer B. (2011). Giriş. In A. A. Hayaloğlu and B. Özer (Eds) Peynir Biliminin Temelleri (pp. 1-8). İzmir, Sidas.
Jiang D, Chen WQ, Zeng X, Tang L. (2018). Dynamic Stocks and Flows Analysis of Bisphenol A (BPA) in China: 2000–2014. Environ Sci Technol, 52: 3706-3715.
Kang JH, Kondo F. (2003). Determination of bisphenol A in milk and dairy products by high-performance liquid chromatography with fluorescence detection. J Food Protect, 66, 1439–1443.
Li J, Zhou H, Liu YX, Yan XY, Xu YP, Liu SM. (2014). Solid-phase extraction for selective determination of bisphenol A in drinks and fruits by dummy surface molecularly imprinted polymer with direct synthetic method. Food Addit Contam, 31: 1139-1146.
Liao C, Kannan K. (2013). Concentrations and profiles of bisphenol A and other bisphenolanalogues in foodstuffs from the United States and their implications for human exposure. J Agr Food Chem, 61: 4655–4662.
Loh SH, Ong ST, Ngu ML, Ariffin MM. (2017). Rapid extraction of bisphenol a by dispersive liquid-liquid microextraction based on solidification of floating organic. Sains Malays, 46: 615-621.
Mercogliano R, Santonicola S. (2018). Investigation on bisphenol A levels in human milk and dairy supply chain: A review. Food Chem Toxicol, 114: 98-117.
Nascimento CF, Rocha FRP. (2018). Spectrofluorimetric determination of bisphenol A in tap waters byexploiting liquid-liquid microextraction in a sequential injection system. Microchem J, 137: 429-434.
Rezaee M, Yamini Y, Shariati S, Esrafili A, Shamsipur M. (2009). Dispersive liquid–liquid microextraction combined with high-performance liquid chromatography-UV detection as a very simple, rapid and sensitive method for the determination of bisphenol A in water samples. J Chromatogr A, 1216: 1511-1514.
Sadeghi M, Nematifar Z, Fattahi N, Pirsaheb M, Shamsipur M. (2016). Determination of bisphenol A in food and environmental samples using combined solid-phase extraction–dispersive liquid–liquid microextraction with solidification of floating organic drop followed by HPLC. Food Anal Methods, 9: 1814-1824.
Santonicola S, Ferrante MC, Murru N, Gallo P, Mercogliano R. (2019). Bisphenol A in cow milk and dietary exposure at the farm level. J Dairy Sci, 102: 1007-1013.
Seachrist DD, Bonk KW, Ho SM, Prins GS, Soto AM, Keri RA. (2016). A review of the carcinogenic potential of bisphenol A. Reprod Toxicol, 59: 167-182.
Staples CA, Dome PB, Klecka GM, Oblock ST, Harris LR. (1998). A review of the environmental fate, effects, and exposures of bisphenol A. Chemosphere, 36: 2149-2173
Sun C, Leong LP, Barlow PJ, Chan SH, Bloodworth BC. (2006). Single laboratory validation of a method for the determination of bisphenol A, bisphenol A diglycidyl ether and its derivatives in canned foods by reversed-phase liquid chromatography. J Chromatogr A, 1129: 145-148.
Turner NW, Subrahmanyam S, Piletsky SA. (2009). Analytical methods for determination of mycotoxins: A review. Analytica Chim Acta, 632: 168-180.
US Environmental Protection Agency (USEPA). (1993). Bisphenol A. (CASRN 80-05-7), integrated risk information system (IRIS). USEPA, Washington, DC. Available from: http://www.epa.gov/iriswebp/iris/subst/0356.htm.
Vandenberg LN, Maffini MV, Sonnenschein C, Rubin BS, Soto AM. (2009). Bisphenol-A and the great divide: A review of controversies in the field of endocrine disruption. Endocr Rev, 30: 75-95.
Vera-Avila LE, Rojo-Portillo T, Covarrubias-Herrera R, Pena-Alvarez A. (2013). Capabilities and limitations of dispersive liquid–liquidmicroextraction with solidification of floating organic drop for theextraction of organic pollutants from water samples. Anal Chim Acta, 805: 60-69.
Welshons WV, Susan CN, vom Saal FS. (2006). Large effects from small exposures. III. Endocrine mechanisms mediating effects of bisphenol A at levels of human exposure. Endocrinology, 147: 56-69.
Wlodarczyk E. (2015). Occurrence of bisphenol A and its effects on the human body. Arch Physiother Glob Res, 19: 13-26.
Yang Y, Yu J, Yin J, Shao B, Zhang J. (2014). Molecularly imprinted solid-phase extraction for selective extraction of bisphenol analogues in beverages and canned food. J Agric Food Chem, 62: 11130-11137.