PH04 Advances in Analysis and Measurements
Exhibit Hall
8:00 AM - Thursday
(PH008) Determination of PCBs, organochlorine and organophosphate pesticides in high lipid fish tissues with NPLC cleanup.
You, J1, Lydy, M1, 1 Southern Illinois University, Carbondale, IL, USA
ABSTRACT- A simple normal phase liquid chromatography (NPLC) method was developed for the simultaneous purification and fractionation of polychlorinated biphenyls (PCBs), organochlorine and organophosphate pesticides in high lipid fish extracts. The two fractions collected after NPLC were analyzed with gas chromatography with an electron-capture detector for PCBs and pesticides, respectively, while two columns were used for the confirmation of the analytes. High lipid fish tissue was sonicated with acetone-hexane (1:1, v/v), and the supernatant was decanted, concentrated and subjected to NPLC with a silica gel column. Ethyl acetate and hexane mixture (1:99, v/v) was used as the mobile phase and two fractions were collected for PCBs and pesticides analysis. The column was cleaned with several injections of ethyl acetate after collection of the desired fractions. High efficiency of elimination of lipid was achieved with this NPLC method so no dilution of sample was required with lipid content less than 20%. The method provided recoveries of 86.8-107.9% for PCBs and 87.3-118.8% for pesticides with relative standard deviations of less than 7%. The method detection limits were at the low ng/g level, and the entire cleanup procedure took only 30 minutes. This NPLC method was compared with sulfuric acid digestion as a possible cleanup technique for the analysis of PCBs in fish and egg samples. The NPLC technique provided clean chromatograms due to the high efficiency of elimination of lipid and the fractionation of PCBs from organochlorine pesticides. The established method was applied to fish tissue samples (filet, brain and gonad) with different lipid content (7-60%).
Key words: polychlorinated biphenyls, normal phase liquid chromatography, organochlorine pesticides, high lipid content sample