Protocol for the determination of selected neutral and acidic semi-volatile organic contaminants in fish tissue.

Progress toward the development of a protocol for the determination of a broad spectrum of organic compounds in fish tissue is reported. Finely ground and homogenized fish tissue samples were Soxhlet extracted. Phenolic compounds in the extracts were acetylated and the derivatized extract containing the acetates and neutral semi-volatiles was cleaned up with silica gel and size-exclusion column chromatography. These semi-volatile organic compounds were determined by gas chromatography-mass spectrometry. The method is evaluated for recovery and precision of selected analytes during the analysis of over 300 fish tissue samples of varying species in support of contaminant determination in fish tissue from the Columbia/Snake River watershed.

Application of polydivinylbenzene liquid chromatography columns to remove lipid material from fish tissue extracts for the analysis of semivolatile organics.

Liquid chromatography columns of 100% polydivinylbenzene (DVB) (packing) were used to remove lipid material from fish extracts before analysis of several semivolatile organic pollutants by gas chromatography-mass spectrometry (GC-MS). This packing material was found to be durable as the columns could be operated to about 900 p.s.i. resulting in high efficiency separation. Recoveries and relative standard deviations for 18 polynuclear aromatic hydrocarbons fortified into a fish extract and cleaned up by multiple DVB columns in series were in the range of 86 to 123% and 4 to 11%, respectively.