| In recent years,food safety issues caused by food contact materials have been occurred repeatedly,and the research on key detection technology for risk substances in food contact materials has gradually attracted more and more attention.According to their functions,the risk substances in food contact materials can be classified into plasticizers,flame retardants,coloring agents,stabilizers,antioxidants and mildew preservatives.Most of the risk substances have had limit values in the domestic and foreign regulations and standards,but the relevant testing standards are still deficient.Therefore,the research on the key detection technology of the risk substances is a significantly important research aspect in food contact materials.Nonylphenol,Bisphenol F and Bisphenol S are acknowledged as endocrine disrupting substances.Owing to its strong environmental estrogenic effect and bioaccumulation,Nonylphenol has been identified as a persistent toxic chemical pollutant.Bisphenol F is an inducement of animal reproduction rate-reduce and germ cell malformation,and Bisphenol S is a threat to infant health.Therefore,these three kinds of high-risk substances mentioned above,Nonylphenol,Bisphenol S and Bisphenol F,have been studied in this paper,and the related detection methods have been established and applied in practice.This research mainly includes the following three parts:1.Development and application of detection method of Nonylphenol in food contact materialsBased on HPLC tandem mass spectrometry,the detection method of content and migration of Nonylphenol in food contact materials is established,and the method has good linear relationship in 0.006~0.3 mg/L range.The detection limit of content Nonylphenol is 2.5 μg/kg,the recovery rate is 89.9%~110.3%,and the relative standard deviation(RSD)(n=6)is 7.4%.The detection limit of the migrated Nonylphenol is 5.0 μg/kg,and the recovery rate is 93.1%~107.1%,RSD(n=6)is 4.6%.In all of the 10 batches of samples,Nonylphenol is not detected in 2 batches,and the contents of Nonylphenol detected in the other 8 batches are between 5.8 to 172.4 μg/kg.The results of migrated amount indicate that Nonylphenol is not detected in 4 batches and the range of migrated Nonylphenol in the other 6 batches is 24.5~83.1 μg/kg.The results show that temperature,migration time is positively correlated to quantity of migration.Moreover,highest quantity of migrated Nonylphenol is found in iso-octane,followed by 95%ethanol,water and 4%acetic acid the minimum.2.Development and application of detection methods of Bisphenol F and Bisphenol S in food contact materialsThe detection method of the content and migration of Bisphenol F and Bisphenol S in food contact materials is established based on HPLC tandem mass spectrometry.This method has good linear relationship in 5~1000 ng/ml range for Bisphenol F and in 2~250 ng/ml for Bisphenol S.The detection limit value of Bisphenol F and Bisphenol S content is 1μg/kg and 6 μg/kg,respectively.The detection limit of migrated amount of Bisphenol F and Bisphenol S is 0.001μg/ml and 0.0005μg/ml,respectively.The recovery rates of Bisphenol F and Bisphenol S are 93.2%~106.3%and 95.6%~107.4%,and the recovery rates of migrated amount of Bisphenol F and Bisphenol S are 95.1%~107.3%and 91.9%~109.2%.The content methods RSD(n=6)for Bisphenol F and Bisphenol S is 4.5%and 3.9%,respectively.The Migration method RSD(n=6)are 4.1%and 5.7%.However,the results show that the migrations of neither Bisphenol F nor Bisphenol S sample were detected in any case of all 10 batches.3.Development and application of material identification of melamineThe characteristic peaks of melamine and urea formaldehyde in Fourier-IR spectra provide a new method for the identification of melamine tableware.This method can efficiently identify the surface and interior substance of melamine tablewares.The results of 80 batches of tablewares collected from the market show that only 21.3%is pure melamine resin tablewares,and 13.7%is urea-formaldehyde-replaced tablewares.The melamine tablewares blending with urea-formaldehyde resin accounts for 2.5%,and 62.5%tablewares are found using urea aldehyde as interior material and coating the surface with melamine resin. |