Determination And Risk Assessment Of Phthalic Acid Esters In Food And Food Packaging Materials

Objective:1.To establish a method for the determination of25phthalate esters in food and food packaging materials.2.To determine and analy assessment the content and the distribution of phthalic acid esters in seven different kinds of food and food packaging materials (beverage,oil and so on) which sell on the market.Methods:1. Method of determination of25kinds of phthalic acid estersThe samples were extracted with n-hexane or n-hexane and acetonitrile by ultrasonic method, purified with solid phase extraction column and eluted with acetonitrile. After drying with water bath nitrogen blowing instrument, the diluted derivatives were separated on HP-5MS column with temperature programming. The identification and quantification of phthalic acid esters were performed by GC-MS in the selected ion monitoring (SIM) mode.2. Determination of phthalic acid esters in7kinds of samplesWe collected a total of281samples of seven categories, including20beverages,27liquors,40vegetables,100oils,12animal visceram,22puffed foods and60food packaging materials. Beverages and liquors were separated by centrifugation or elimination of carbon dioxide, and then extracted with n-hexane; Vegetables were extracted with sodium chloride and n-hexane by ultrasonic method three times respectively, and the supernatant was concentrated by rotary evaporation after centrifugation; oils, animal viscera and puffed food were extracted with n-hexane or n-hexane and acetonitrile, and then the acetonitrile layer was purified with solid phase extraction column, eluted and dried with nitrogen blowing instrument; food packaging materials were extracted with n-hexane three times and the extracts were concentrated.3. Survey of the dietary consumptionAdopting multistage and stratified sampling, a total of1104residents in Qingdao were adopted for investigation of24-hour dietary questionnaire. We collected six categories of food consumpution for three consecutive days and recorded consumption with data entry bookkeeping. 4. The result of analysisWe calculate the content of25kinds of phthalic acid esters in these samples, performed chi-square test and then analysis of variance with spss17.0analysis software in order to analyze the content distribution of phthalic acid esters in different varieties, places and seasons.Using the point evaluation method, the health risks index (HI) of food dietary intake of PAEs and risk assessment. Calculate health risk index (HI) in six food dietary intake of PAEs and assess risk.Results:1The limits of detection of25kinds of phthalic acid esters were from0.002mg/kg to0.050mg/kg (S/N=3). The average recovery was85.2%～108%and the precision ranged from1.8%to7.6%.2Content distribution of phthalic acid esters in different varieties2.1Comparison of detection rate of different phthalates in different samplesIt can be concluded that the detection rates of DEHP was high, and the differences were statistically significant in different varieties (χ2=90.36,P<0.001); the detection rates of DBP was statistically significant in different varieties(x2=57.51,P<0.001); the detection rates of DIBP was statistically significant in different varieties (χ2＝41.47, P<0.001); the detection rates of DMP was statistically significant in different varieties(x2=25.06,P=0.001).2.2Comparison of content distribution of phthalic acid esters in different categories and sampling methodsThe contents of DEHP were remarkably different in different types of cooking oil(F=7.411,P=0.000) and in different sampling sites of cooking oil(F=3.315, P=0.023).Significant differences of DIBP and DBP contents were found in different years of liquor (F=6.966,P=0.004;F=3.667,P=0.039,respectively). There were statistically significant difference of the content of DBP and DEHP in different season vegetables(F=3.819,P=0.010; F=5.287,P=0.002),There were statistically significant difference of the content of DEHP, DBP and DIBP in different animal’s gut(F=8.179,P=0.006;F=14.333,P=0.001; F=8.179,P=0.006).There were statistically significant difference of the content of DBP and DIBP in different food packaging materials(F=5.295,P=0.003; F=3.491,P=0.021).There were statistically significant difference of the content of DIBP in different sampling sites of PVC(F=4.156, P=0.032).3Six types of food intake of risk assessment3Health risk index (HI) of PAEs in peanut oil was less than one, which was at low risk. Although average consumption of vegetables daily was the biggest, HI of PAEs in vegetables sustained at extremely low levels which was less than one and was considered low risk. The similar results were found in other food with HI of PAEs less than one, which suggested they displayed lower risk.Conclusions:1This method is fast, stable and simple, with high average recovery rate. The high sensitivity, precision and accuracy of the method can meet the testing requirements for the qualitative and quantitative determination.2The type and content of phthalic acid esters varies in different foods, sampling sites and seasons.3Nowadays, the pollution of phthalic acid ester has covered most of the food. According to the content of phthalic acid esters, we can find that it is impossible to add intentionally, and there is no risk for people’s daily life for now. But we should further research whether long-term phthalic acid ester pollution impact on humans.