Method For Determination Of Environmental Hormones Of Phthalate Acid Esters In Food Plastic Packaging Materials

Phthalate acid esters are worldwide pollutants, also typical environmental hormones. It may affect human on their normal endocrines by breathe,skin contact and food, leading to reproductive, developmental and behavioral disorder. Phthalate acid esters are widely used as plasticizers in the manufacture of plastics, so it's very necessary to analyze phthalate acid esters in plastics. But there are some weakness in lacking of national reference materials,purifying process after sample pretreatment and controlling matrix effect from complex samples. Instrument will be polluted easily when samples were injected directly without purification. The paper do some research aiming at such questions:1. Developed national reference materials of phthalate acid esters, including six phthalate acid esters such as DMP, DEP, DIBP, DBP, DEHP and DOP. At the same time analytical method used to analyze these compounds will be founded. And this paper established different methods such as GC and HPLC served to develop national reference materials.2. Explored new sample pretreatment methods: The thesis has established the preparation method with soxhlet extraction with Foss soxtec 2050.And hexane is used as extraction solvent and rinse time is sixty minutes after a series of experimentations. After soxhlet extraction, solid phase extraction has be done to purify sample solution. Three key factors such as rinse solvent, elute solvent and elute volume are optimized. Hexane and toluene (their volume ratio is one to one) are used as rinse solvents, two milliliter ethyl acetate is used as eluting solvent. And then it can be found that there are less impurity in samples which analyzed by GC.3. The average recoveries of thirteen phthalate acid esters are from 70% to 130%. And relative standard deviations (n=6) of higher concentration is from 2.8% to 8.7%, and the lower concentration from 1.0% to 6.7%. The method detection limits of these compounds are from 0.005 to 0.03μg/g.4. Sumed up fragmentation regularity of PAEs by analyzing fragment ion of each compound, and we know fragmentation pathway of m/z149.