Westbom Rikard, Thörneby Lars, Zorita Saioa, Mathiasson Lennart, Björklund Erland
Department of Analytical Chemistry, Lund University, P.O. Box 124, S-221 00 Lund, Sweden.
J Chromatogr A. 2004 Apr 9;1033(1):1-8. doi: 10.1016/j.chroma.2004.01.022.
Polychlorinated biphenyls (PCBs) in water were extracted with a rebuilt extraction unit using 47 mm C18 solid-phase extraction (SPE) disks. Three types of disks (SPEC, ENVI and Empore) were investigated for the extraction of seven PCBs from 11 reagent water spiked at two concentration levels (20 and 1000 ng/l). The Empore disks produced the best analyte recoveries (91-107% with R.S.D. of 1-8%) at the low concentration level and displayed no leaking tendency. Empore disks were therefore considered superior to ENVI and SPEC disks for the conditions outlined in this work. The obtained extracts were dried and purified in an additional clean-up step using custom-made columns containing Florisil and Na2SO4. For water containing large amounts of organic matter, a pre-filtration was included. Final analysis was carried out on a dual-column GC-electron-capture detection system with on-column injection. The optimised extraction method, including clean-up, was less time-consuming and used less hazardous organic solvents than conventional liquid-liquid extraction (LLE) methods. Recoveries were 92-102% with R.S.D. of 3-8%.
使用配备47毫米C18固相萃取（SPE）盘的改装萃取装置提取水中的多氯联苯（PCBs）。研究了三种类型的萃取盘（SPEC、ENVI和Empore）从两种浓度水平（20和1000纳克/升）加标的11份试剂水中萃取7种多氯联苯的情况。在低浓度水平下，Empore萃取盘的分析物回收率最佳（91 - 107%，相对标准偏差为1 - 8%），且无渗漏倾向。因此，对于本工作所述条件，Empore萃取盘被认为优于ENVI和SPEC萃取盘。所得提取物在额外的净化步骤中使用装有弗罗里硅土和硫酸钠的定制柱进行干燥和净化。对于含有大量有机物的水，进行了预过滤。最终分析在带有柱上进样的双柱气相色谱 - 电子捕获检测系统上进行。与传统液 - 液萃取（LLE）方法相比，包括净化步骤在内的优化萃取方法耗时更少，且使用的有害有机溶剂更少。回收率为92 - 102%，相对标准偏差为3 - 8%。
