水产品中邻苯二甲酸酯类增塑剂存在状态研究及其双水相提取测定  

Investigation on the form of phthalates in aquatic products and its efficient extraction and detection by aqueous two phase system

作　　者：王文文[1] 李桂芝[1] 王翠霞[1] 刘振波[1] 刘永明[1] 

机构地区：[1]烟台大学化学化工学院,山东烟台264005

出　　处：《化学研究与应用》2013年第1期27-32,共6页Chemical Research and Application

基　　金：国家自然科学基金项目(20973149)资助;山东省自然科学基金项目(ZR2011BM009)资助

摘　　要：利用荧光猝灭法与GC-MS研究了邻苯二甲酸酯类(PAEs)在以蛋白质为主要基质的水产品中的存在状态,探讨了蛋白质对PAEs萃取率的影响。结果表明,PAEs可通过氢键和范德华力与蛋白质牢固结合;体积分数为80%的异丙醇水溶液可引起蛋白质缓慢变性、使结合的PAEs充分离解,通过异丙醇-无机盐-水双水相体系实现PAEs的高效萃取。由于80%的异丙醇水溶液极性较强,与PAEs共同进入双水相上相的脂溶性杂质较少,萃取液净化步骤大大简化。在双水相上相中加入无水MgSO4、N-丙基乙二胺(PSA)去除水分与杂质后直接进样进行GC-MS检测。该方法用于水产品中五种PAEs的测定,回收率为81.9%～92.7%,相对标准偏差为1.2%～4.8%。The fluorescence quenching method and C,C-MS were applied to study the form of PAEs in protein matrix of aquatic prod- ucts. Meanwhile, the influence of the protein on extraction of PAEs was investigated in detail. The results showed that PAEs strongly bound with BSA by the hydrogen bond and Van der Waals force. In the φ （2-propanol）80% aqueous solution protein denaturation could occur and the PAEs binding with the protein could be dissociated fully. Following the PAEs was extracted by aqueous two phase system with high extraction efficiencies. Owing to the high polar of φ （2-prepanol） 80% aqueous solution,less fat-soluble sub- stance was extracted and the purification steps were greatly simplified. The anhydrous magnesium sulfate（ MgSO4 ）and primary sec- ondary amine（PSA） were added in upper phase to eliminate the moisture and other impurities. Then, the PAEs in extract （upper phase） was directly analysed by GC-MS. The accuracy of this method was evaluated by measuring the recovery from spiked samples. Overall recoveries were 81.9～92. 7%with RSD values of 1.2～4.8%.

关 键 词：邻苯二甲酸酯 双水相 蛋白质 异丙醇 气相色谱-质谱法 

分 类 号：O657.3[理学—分析化学]