Studies On Analytical Method Of The Trace PCBs In Fish Oil

In this paper, accurate analysis method of trace deleterious PCBs infish oil has been investigated to cover the shortage in our country, andpretreatment and accurate determination method of the samples havebeen set up. Firstly, the method using gel permeation and Florisil columnchromatographic clean-up techniques for the determination of residues ofPCBs in fish oil is investigated and established. GPC is a non-destructivelipid removal method, can be fully automated, and the reagent used in thisexperiment has low toxicity. The experimental results indicate that theefficiency of lipid removal of the established method is 99.9% and therecovery of the method is 87%~95%. The RSD of the repeating recoveryexperiments is 1%~2%. In addition, The method of using subsection SIM of GC/MS inqualitatively and quantitatively analyzing PCBs in fish oil samples is builtup. The selectivity of the method is high and the detection limit of iii北京化工大学硕士学位论文analyzing PCB reference sample is 0.1~1pg (SNR is 2). The RSD ofrepeatedly analyzing PCB reference sample is 0.1%~0.7%. the methodof analyzing PCBs by GC/MS is also investigated and established. It hasshown that when using this method in analyzing PCBs mixed criterionsample, the effect of separating PCBs is very good. Next, a non-spiked fish oil sample is analyzed using the establishedclean-up and detection method. It has been found that in this sample,there are 31 kinds of PCBs congeners. The quantitative analysis for 7kinds of PCBs congeners(28, 52, 101, 118, 138, 153, and 180) which areused to monitor PCBs occurrence and distribution in the environment hasbeen done. The result of analysis is that the total concentration of these 7kinds of PCBs congeners is 61ng/mL. It can well indicate that theestablished clean-up and detection method can be used in qualitativelyand quantitatively analyzing PCBs in fish oil sample so that it haspotential application. Finally, the method using concentrated sulphuric acid topurify samples is preliminarily studied. The result of theexperiment indicates that the recovery of PCBs is 88%~96%, andconcentrated sulphuric acid is less devastating to the 10 kinds ofPCBs congeners in PCB reference sample. So it is acceptable to be iv北京化工大学硕士学位论文used in the pretreatment of samples.