亚临界水萃取-高效液相色谱法测定聚碳酸酯水杯中双酚A和苯酚的迁移量  

Simultaneous determination of the migrations of bisphenol A and phenol in polycarbonate bottles based on subcritical water extraction and high performance liquid chromatography

作　　者：白玮玮[1] 刘书慧[1] 曹江平[1] 范盈盈[1] 解启龙[1] 

机构地区：[1]西北农林科技大学理学院,陕西杨凌712100

出　　处：《色谱》2013年第3期254-259,共6页Chinese Journal of Chromatography

基　　金：西北农林科技大学人才专项项目(Z111021005)

摘　　要：建立了亚临界水萃取-高效液相色谱同时测定聚碳酸酯(PC)水杯中双酚A和苯酚迁移量的方法。选择萃取温度120℃、萃取压力6.89 MPa(1 000 psi)、静态萃取时间1 h、萃取1次对11种样品进行测定。双酚A的迁移量为6.81～11.16μg/g。5种样品中未检出苯酚,其余样品中苯酚迁移量为3.25～6.08μg/g。在优化的测定条件下,双酚A和苯酚在8 min内达到基线分离。双酚A和苯酚分别在0.05～20 mg/L和0.02～20 mg/L范围内线性关系良好,相关系数(r)均大于0.999 7,检出限分别为7.6μg/L和2.0μg/L。日内及日间的重复性(以RSD计)分别小于5.21%及11.63%。传统的浸提法结果表明长时间浸提会使PC材料发生微弱水解。相比传统的浸提法,该方法的萃取效率提高了49～106倍。该方法简便、快速、环保,可用来测定PC水杯中双酚A和苯酚的迁移量。A new method was established for the simultaneous determination of the migration amounts of bisphenol A （BPA） and phenol from polycarbonate （PC） bottles based on subcritical water extraction （SWE） and high performance liquid chromatography. The optinmm extraction conditions included an extraction temperature of 120℃：, a pressure of 6. 89 MPa （ 1 000 psi）, a static extraction time of 1 h and one cycle. Under the conditions, the migration amounts of the BPA ranged from 6. 81 to l 1. 16 μg/g in 11 samples. Phenol was not detectable in 5 samples, and in other ones the migration amounts of phenol varied in the range of 3.25 -6.08 μg/g. The traditional soaking extraction experiments showed that PC was subjected to weak hydrolysis after long-time leaching. The BPA and phenol were separated in 8 min. Good linearities were obtained in the range of 0. 05 - 20 mg/L for BPA and 0.02 - 20 mg/L for phenol （ r 〉 0. 999 7 ）. The limits of detection were 7.6 μg/L for BPA and 2.0 μg/L for phenol. Intra-day and inter-day repeatabilities （ expressed as RSD） were less than 5.21% and 11.63%, respectively. Compared with traditional water soaking extraction, the extraction efficiencies increased 49 - 106 times using this developed SWE method. The procedure is simple, rapid and enviromnent friendly, and can be utilized to determine the migration amounts of BPA and phenol in PC bottles.

关 键 词：亚临界水萃取 高效液相色谱 双酚A 苯酚 聚碳酸酯水杯 

分 类 号：O658[理学—分析化学]