| Background Phthalate acid esters (PAEs), also known as phthalate esters, are thegenerally colorless, oily viscous liquid. As PAEs just joined together with plastic hostby the hydrogen key and van der Waals force, they keep each other relativelyindependent chemical properties. It will be dissolved out in suitable organic solventand cause pollution to the environment, living beings and food. The more PAEs is inthe experiental plastic material, the more dissolution. Although the experiental plasticmaterial is almost always used in the experiments, few people are acquainted withPAEs migration and pollution to samples. It’s necessary to research this to avoidlaboratory samples pollution lead to interfere with the results.Intention The purpose of this study is to research the migration problem of PAEs inthe experimental plastic material and investigate a fast and high-efficiency methodsfor extraction, purification of DBP. It has been carried on the all-round appraisal aboutthe structure of DBP by NMR technology. Besides, this provides a preliminaryanalysis on DBP structure.Technique Taking the experimental plastic material as the research object, it providesa preliminary analysis on PAEs in experimental plastic material by thin layerchromatogrpahy. The column chromatography and HPLC technology are used toseparate and purify DBP, in addition, it has been carried on the all-round appraisalabout the structure of DBP by NMR technology. It can estimate other basic migrationlaws of PAEs by the analysis about DBP migration which provides a reference for thefuture similar study.Result1After the HPTLC analysis of the PAEs in plastic material, the RF Value of DBPwas0.51, proportion accounts for10.39%under the292nm detection wavelength.2The column chromatography separation conditions of DBP has been exploredand optimized. Ultimately, the mixture of petroleum ether and ethyl acetate was adopted, and then can get the crude DBP with the mixture of petroleum ether andethyl acetate in the ratio of1:3. The purity of the crude DBP can reach more than45%detected by HPTLC, greatly improving the purification and concentration levels.3In the DBP purifying phase, the extracts were disposed by preparation of thinlayer chromatography and high performance liquid chromatography, compared theadvantages and disadvantages of two methods. Ultimately, PHPLC technology wasadopted for purification.The purity of the purified DBP sample can reach97.51%±0.933%detected by HPLC. Repeatability test is carried out for the HPLC detectionlevel, then it was good that the purified DBP RSD of retention time and peak area wasless than2%. It has been carried on the all-round appraisal about the structure of DBPby NMR technology.4During the migration process, three main factors including migration solvent，time, temperature, were studied by using single factor analysis method. According tothe experimental results, ingredients could be dissolved in five migration solvent.Total migration amount in turn was: petroleum ether> chloroform> ethylacetate>ethanol> methanol, in addition, the migration amount increase with the increase oftemperature, soaking time within certain realms.Conclusion and InnovationDifferent elution systems were selected by TLC and column chromatography toestablish the preliminary separation and purification methods of the PAEs in plasticmaterials. It has good dyeing effect for DBP by the improved bismuth potassiumiodide and therefore. It was intuitive and easy to see separations of various kinds ofPAEs on the thin layer analysis. It has carried on the all-round appraisal about thestructure of DBP by NMR technology.It showed that the PAEs in plastic material were dissolved in different degreeswhich may damage to the test samples in different organic solvents, different time,different temperature by the migration experiment. So try not to use plasticconsumables consumables to storage test samples in laboratory tests. |
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