| Phthalate esters are a common type of plastizer which have been widely used as additives in a number of light industry products,such as toys,food packaging,detergents,lubricants,personal care products and so on.The main function of phthalate esters is to soften the vinyl.Therefore,they can increase the ductility and softness of polymer materials,change hard plastic into a flexible plastic,and not affect the durability of plastics,as well as improve the strength of plastic products,they are widely used in.There are no covalent bonds fromed among phthalate esters plasticizer and/or the plastics,therefore the added phthalate esters are in the free styles,and still retain their relatively independent chemical properties.When the phthalate esters in plastics contact with the packaging substances such as water,grease and others,they can be easily dissolved,migrated from the plastics into the external environment,which resulting in air,water,soil and food contaminations as time goes on.Since phthalates are difficult to degrade in the environment,they have become one of the most common environmental pollutants in the world.During the past decades,many detection methods and testing standards have been developed for the determination of phthalate esters,however,they still are not cover all toy materials.Moreover,some of these methods involvedthe use of environmentally unfriendly and toxic reagents.The aim of this study is to develop an accurate,efficient,safe and fast method for determination of phthalate esters in toy materials.In part I,according to the detection standard of phthalate esters at home and abroad,combined with instrument and equipment conditons in our laboratory,a method for simultaneous determination of 6 kinds of different phthalate esters(DBP,BBP,DEHP,DNOP,DINP,DIDP)by gas chromatography-mass spectrometry(GC-MS)was firstly established.All 6 phthalate esters and DAP of the internal standard have reached the baseline separation requirement.Then weverify the standards,such as SN/T 2249-2009-Determination of phthalates inplastics and plastic articles-Gaschromatography-massspectrometry(GC-MS)method,EN14372-2004-Child use and care articles-Cutlery and feeding utensils-Safety requirements and tests etc.The feasibility,rationality and accuracy of these standards were also evaluated.In part II,the effects of solvents on the the extraction efficiency of phthalate esters in five different kinds of toy materials,including leather,textiles,PVC,rubber and paint,have been investigated.These extraction solvents includedn-hexane,iso-octane.The results revealed that the highest extration efficiency for the phthalate esters extraction in leather materail was obtained by using solvent mixture n-hexane:acetone(1:1)as extraction agent.Whilst,the solvent ethyl acetate achieved the highest extration efficiency for the phthalate esters extraction in textiles,polyvinyl chloride,rubber and paints materails.By referencing to domestic and international standards,the effects of extraction methods on the extraction efficiency of phthalate esters in toys were also investigated.The results showed that Soxhlet extraction method achieved the highest extration efficiency for leather materail,and microwave extraction method achieved the highest extration efficiency for textiles,polyvinyl chloride,rubber and paint materials.For Soxhlet extraction method,an increased extraction efficiency could be obtained by prolonging the extraction time to six hours.For microwave extraction method,increasing the microwave extraction temperature to 100 ~oC could impove the extraction efficiency.In this study,the effects of 12 kinds of solvents and 4 kinds of extraction ways on the extraction efficiency for phthalate esters extraction in five different kinds of toy materials,including leather,textiles,PVC,rubber and paints,have been compared and investigated for the first time. |
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