【作者】 张颖；

【导师】 陈伟；

【作者基本信息】 山东农业大学 ， 食品加工与安全（专业学位）， 2017， 硕士

【摘要】 全氟化合物(Perfluorochemicals,PFCs)是一类持久存在于环境中的新型有机污染物。近年来,大量的研究显示,全氟化合物已被发现在食品、土壤、水、空气、接触材料等介质中。由于PFCs在环境的长久污染性和在生物体内的积累性,使其越来越受到人们的关注。由于近几年中国的氟化工行业的快速发展,在中国一些城市的饮用水污染现状均高于其他国家。所以在食品安全领域对水中痕量全氟类化合物的分析测定一直是研究的热点。在本研究中,使用了一种表面经羧基修饰过的新型功能化纳米碳球-羧基化纳米碳球(CNSs-COOH),使之作为固相萃取(SPE)吸附剂,联合液相色谱串联质谱仪(LC-MS/MS)建立了一种测定水中六种全氟类化合物的新方法,并对不同地方的实际水样品基质进行了检测分析,验证了该方法的实用性。本研究主要结果如下:1.通过对萃取条件(萃取时间、pH值)、解吸条件(解吸溶剂种类、解吸溶剂体积)、水样品的体积及羧基化纳米碳球的用量进行优化等条件优化,得到了最优实验条件为:400 mL pH=2的水样品,流速为6 mL/min,解吸溶剂为pH=10的丙酮7 m L,羧基化纳米碳球用量为300 mg。2.在最优实验参数下,建立的方法对于全氟癸酸(PFDA)、全氟壬酸(PFNA)、全氟辛酸(PFOA)、全氟庚酸(PFHpA)、全氟己烷磺酸(PFHxS)和全氟辛烷磺酸(PFOS)拥有0.01~1.20 ng L-1的低检出限,在0.5~200 ng L-1的线性范围内线性关系良好,相关系数(R2)为0.997~0.999,相对标准偏差介于3.70~8.80%。3.该方法被应用于桶装饮用水、自来水及池塘水样品的分析检测,在自来水样品中有PFHxS被检测出,在池塘水样品中有PFHxS和PFOS被检测出,而在桶装饮用水中6种全氟类化合物均未被检出。在100 ng L-1、50 ng L-1、10 ng L-1三个浓度下加标试验,回收率为82.2~109.7%。更多还原

【Abstract】 Perfluorochemicals are persistent in the environment of new organic pollutants.In recent years,Perfluorochemicals have been found in food,soil,water,air,contact materials and other media through a large number of research.More and more people has been focued on Perfluorochemicals because of the long-time existence of PFCs in the environment and the accumulation in organisms.In recent years,China’s fluorine chemical industry’s rapid development,the pollution situation of Perfluorochemicals in drinking water in some Chinese cities is higher than that in other countries.Therefore,It is a hot research topic for Analysis of Trace Perfluorochemicals in water samples in the field of food safety.Carboxylated solid carbon spheres as novel solid phase extraction absorbent for Analysis of Trace Perfluorochemicals in water samples using LC-MS/MS was estiblished.The practicality of the method is verified by detecting the actual water in different places.The main results were as follows:1.The optimal conditions were obtained by optimizing the extraction conditions(extraction time,pH value),desorption conditions(desorption solvent type,desorption solvent volume),water sample volume and Carboxylated Nano-Carbon Spheres quality.And the optimal conditions were as follows: volume of sample,400 m L;pH of sample,2;flow rate of sample,6 m L/min;eluent was 7 mL of pH=10 ACE;CNSs-COOH quality was 300 mg.2.Under the optimized conditions,the detection limits obtained for PFHpA,PFOA,PFNA,PFDA,PFHxS and PFOS were 0.01~1.20 ng L-1.A good linearity over the range 0.5~200 ng L-1 and R2(0.997~0.999)were obtained.3.The method is applied to bottled drinking water,tap water and pond water sample analysis detection,PFHxS were detected in tap water samples,in the pond water samples have PFHxS and PFOS are detected,and the barreled drinking water six Perfluorochemicals were not achieved.The recovery was 82.2~109.7 % in the three concentrations(100 ng L-1、50 ng L-1、10 ng L-1).更多还原