Fujita Hiroyuki, Honda Katsuhisa, Hamada Noriaki, Yasunaga Genta, Fujise Yoshihiro
Department of Environmental Science for Industry, Ehime University, 3-5-7 Tarumi Matsuyama, Ehime 790-8566, Japan.
Chemosphere. 2009 Feb;74(8):1069-78. doi: 10.1016/j.chemosphere.2008.10.053. Epub 2008 Dec 17.
Validation of a high-throughput measurement system with microwave-assisted extraction (MAE), fully automated sample preparation device (SPD), and gas chromatography-electron capture detector (GC-ECD) for the determination of polychlorinated biphenyls (PCBs) in minke whale blubber was performed. PCB congeners accounting for > 95% of the total PCBs burden in blubber were efficiently extracted with a small volume (20 mL) of n-hexane using MAE due to simultaneous saponification and extraction. Further, the crude extract obtained by MAE was rapidly purified and automatically substituted to a small volume (1 mL) of toluene using SPD without using concentrators. Furthermore, the concentration of PCBs in the purified and concentrated solution was accurately determined by GC-ECD. Moreover, the result of accuracy test using a certified material (SRM 1588b; Cod liver oil) showed good agreement with the NIST certified concentration values. In addition, the method quantification limit of total-PCB in whale blubbers was 41 ng g(-1). This new measurement system for PCBs takes only four hours. Consequently, it indicated this method is the most suitable for the monitoring and screening of PCBs in the conservation of the marine ecosystem and safe distribution of foods.
对一种高通量测量系统进行了验证,该系统采用微波辅助萃取(MAE)、全自动样品制备装置(SPD)和气相色谱 - 电子捕获检测器(GC - ECD)来测定小须鲸鲸脂中的多氯联苯(PCBs)。由于同时进行皂化和萃取,使用MAE用少量(20 mL)正己烷就能有效地萃取出占鲸脂中总多氯联苯负担95%以上的多氯联苯同系物。此外,通过MAE获得的粗提取物使用SPD快速纯化并自动置换为少量(1 mL)甲苯,无需使用浓缩器。此外,通过GC - ECD准确测定了纯化和浓缩溶液中多氯联苯的浓度。而且,使用认证物质(SRM 1588b;鳕鱼肝油)进行的准确度测试结果与美国国家标准与技术研究院(NIST)认证的浓度值吻合良好。另外,鲸脂中总多氯联苯的方法定量限为41 ng g(-1)。这种新的多氯联苯测量系统仅需四个小时。因此,这表明该方法最适合在海洋生态系统保护和食品安全分配中对多氯联苯进行监测和筛选。