Abstracts / Toxicology Letters 205S (2011) S60–S179
P1265 Determination of melamine in milk and dairy products by HPLC A. Filazi 1,∗ , U.T. Sireli 2 , H. Ekici 1 , H.Y. Can 2 , A. Karagoz 2
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and 25% for the intraday and interday precision, respectively. The triple quadrupole (QqQ) analyzer simultaneously operated in the selected reaction monitoring (SRM) and selected ion monitoring (SIM) modes, acquiring two or three transitions per compound. The method has been successfully applied to the analysis of pesticide residues in 25 real honey samples.
1
Department of Pharmacology and Toxicology, Ankara University Faculty of Veterinary Medicine, Diskapi-Ankara, Turkey, 2 Department of Food Hygiene and Technologies, Ankara University Faculty of Veterinary Medicine, Diskapi-Ankara, Turkey
Melamine is produced in large amounts primarily for use in the synthesis of melamine formaldehyde resins for the manufacture of laminates, plastics, coating, commercial filters, glues and dishware. It has high nitrogen content and is added to milk to mask the low protein content. It has low acute toxicity, whereas chronic exposure to melamine may cause to several organs damage and even death. This present survey was aimed to find out if the Turkish people are exposed to melamine by milk and dairy products. For this, domestic and imported milk and dairy products (n = 300) were purchased from national chain grocery stores in Ankara, Turkey, between 1 and 30 June 2010. Melamine concentrations were determined by HPLC with diode array detector. According to the results, melamine was not found in infant formulas and pasteurized/UHT milk, whereas in 2% of spreadable cheese (one sample), 8% of milk powder (4 samples) and 48% of fruit yogurt (24 samples) contained melamine in 1.21 ppb, 0.07 A˚ ± 0.01 ppb (0.05–0.09 range), 2.78 A˚ ± 1.3 ppb (0.07–4.79 range) levels, respectively. These findings were below the limits, set by Codex Alimentarius Commission and EU Legislation (1 ppm for infant formula, 2.5 ppm for dairy products). It could be assumed that the lower amounts are due to the contamination during the preparation of dairy products and the higher amounts are due to the deliberate addition. Therefore, it is considered that the consumption of foods containing these low levels of melamine does not constitute a health risk for consumers. doi:10.1016/j.toxlet.2011.05.499
P1266 Multiresidue analysis of pesticides in honey by quechers and gas chromatography mass spectrometry in tandem G. Font ∗ , E. Ferrer, H. Berrada Laboratory of Toxicology, Faculty of Pharmacy, University of Valencia, Burjassot, Spain A rapid multi-residue method has been developed for the determination of 20 pesticide residues in honey by gas chromatography coupled to triple quadrupole mass spectrometry using a quick, simple, inexpensive and effective sample preparation. Honey is an important product consumed as a dietary supplement by humans due to its high contents of nutrients and can be also important source of pollutants and pesticides. The method is based on the modified QuEChERS sample preparation method. 10 g of sample was shacked with 10 mL of acetonitrile containing1% of acetic acid, followed by a liquid–liquid partition formed by the addition of 4 g of MgSO4 and 1 g of NaOAc. Then, 150 mg of MgSO4 and 25 mg of primary secondary amine (PSA) were added to 1 mL of organically phase and shacked vigorously 1 min, centrifuged, filtered and injected at the GC–MS/MS system. The method has been properly validated in a wide dynamic range (20–500 g kg−1 ): Recovery was studied at three concentration levels (20, 50.0, and 150.0 g kg−1 ), yielding values in the range 68–1070% with precision values, expressed as relative standard deviation (RSD), lower than 20
doi:10.1016/j.toxlet.2011.05.500
P1267 Solvent and matrix effect on the determination of synthetic food colours in soft drinks M. Goumenou D’ Division of Athens, Department B’ – Food Additives, General Chemical State Laboratory, Athens, Greece The addition of synthetic dyes (SD) in several foods is a common practice around the world. In EU countries only 12 of these dyes are permitted and their use is governed by rules regarding the kind of food and the quantity permitted. Consequently, the accurate determination of SD during the EU market surveillance for safety reasons is imperative. Soft drinks are one widely consumed often colored food. The determination of dyes in soft drinks presents difficulties as the acidic environment of the analytes affects their chemical behaviour. The purpose of this study is to examine solvent and matrix effects on the determination of these 12 SD in soft drinks. For the purpose of this study spiked soft drinks were prepared adding E102, E104, E110, E122, E123, E124, E127, E129, E131, E132, E133 and E142 in commercial soft drinks (one uncolored, one with orange juice and the latter spiked with preservatives) as well as in water. The preparations were analyzed with HPLC–DAD after extraction with water, phosphate buffer (pH 8.0), NH3 /H2 O 0.5% (pH 10.9) and NH3 /H2 O (pH 8.1). Recoveries for all dyes were calculated and compared. The determination accuracy for the yellow and red dyes was significantly better when NH3 /H2 O solution was used. Blue dyes alteration by NH3 /H2 O solution was significant so the phosphate solution is a better choice. These differences are attributed to drift of the spectrum maxima. Minor differences were observed between different soft drinks while the presence of preservatives does not seem to affect the dyes’ determination. doi:10.1016/j.toxlet.2011.05.501
P1268 Evaluation of total arsenic content in chicken heart and liver. A comparative approach C.M. Gutu 1,∗ , M. Ilie 1 , V. Preoteasa 2 , M. Gubandru 1 , D. Balalau 1 , G. Manda 2 1
Toxicology, Carol Davila University of Medicine and Pharmacy Faculty of Pharmacy, Bucharest, Romania, 2 Radiobiology, Victor Babes National Institute, Bucharest, Romania Purpose: Chicken meat is exposed to arsenic contamination, generally due to growth additives in feed, even if that is forbidden in several countries. Consequently, the evaluation of arsenic level in meat is of great importance. The study aims to compare different methods to assess the arsenic level in chicken heart and liver using atomic absorption spectroscopy (AAS). Methods: Commercially available chicken liver and hearts from Romanian farms were taken into consideration. The tissue was homogenized, mineralized using microwave digestion, and analyzed via AAS using the