Analyses were replicated to validate the precision of 

 the analysis. Agreement among triplicate samples 

 extracted on the same day was ±5% of the mean. A 

 sample was fortified with 1.0 ppm Aroclor 1254 each 

 week to check percent recovery. The spiking solution 

 was pipetted directly onto the homogenized flesh 

 contained in the blender jar and worked up by AOAC 

 multiresidue procedure. Check of final recovery pre- 

 cision was ±11% of the mean. Degradations of 

 specified Aroclors 1242, 1254, and 1260 were mon- 

 itored by running standard mixtures of the com- 

 pounds through the entire procedure in the absence 

 of any sample material. This was done whenever new 

 materials or reagents were used. 



Validation studies were accomplished at the 1.0, 

 0.5, and 0.1 ppm levels. Recovery efficiency for seven 

 samples spiked at the 1.0 ppm level was 83.88%. At 

 the 0.5 ppm level recovery was 85.66%, and at 0.1 

 ppm, 79%. Coefficient of variation ranged from 6.9 to 

 11.5 for the three levels. In addition, a blind sample of 

 homogenized carp was introduced into the sampling 

 system periodically. This sample was provided and 

 thoroughly analyzed by J. D. Petty of the Fish and 

 Wildlife Service, Columbia National Fisheries Re- 

 search Laboratory, Columbia, Mo. 



Finally, the Gloucester Laboratory participated in 

 the ICES 5 fourth organochlorine intercalibration ex- 

 ercise for unspiked and spiked fish oils. The accuracy 

 and precision of the Gloucester Laboratory exceeded 

 the performance level accepted by ICES. 



Confirmation of PCB's by GC-MS 



A 12 m by 0.21 mm i.d. fused silica column (OVID- 

 101) was coupled to a Hewlett-Packard 5992 B GC- 

 MS (gas chromatography-mass spectrometry) and 

 operated in the selected ion monitoring mode. Four 

 extracts of striped bass and four extracts of white 

 perch were analyzed by GC-MS to confirm the pres- 

 ence of chlorosubstituted biphenyls. Ion masses of 

 235, 246, 263, 292, 326, and 360 were selected. In 

 this manner, tetrachloro, pentachloro, hexachloro, 

 heptachlorobiphenyls, aldrin, analogues of DDT, 

 and p,p'-DDE could be detected. The presence of 

 chlorosubstituted biphenyls (4, 5, 6, and 7) was in- 

 dicated. Also, mass spectra of some of the individual 

 peaks were obtained and stored during production of 

 a total ion chromatogram. Subsequently, the in- 

 dividual peaks were identified by comparing their 



5 ICES (International Council for the Exploration of the Sea). An in- 

 tercalibration exercise on PCB's in biological materials carried out 

 by 24 participants using unspiked and spiked samples of cod liver oil 

 to determine agreement among analysts. 



392 



spectra with those in the system's library using a li- 

 brary search program. 



Results 



Table 2 gives the mean PCB concentrations (ppm, 

 wet weight), lipid content, length, weight, age, num- 

 ber of samples, and location for each of the species. A 

 total of 270 samples were analyzed by the AOAC pro- 

 cedure with additional cleanup by silicic acid 

 chromatography. PCB's were detected for all of the 

 samples analyzed. Total PCB values of marine finfish 

 averaged 0.33 ppm, well below the FDA limit of 5 

 ppm and 3/20 of the proposed 2 ppm standard. 



The highest concentration measured in any species 

 was 22.0 ppm in a white perch sampled from the Hud- 

 son River. White perch sampled from Cape May 

 Peninsula had an average total PCB content of 0.06 

 ppm. The Hudson River is known to be heavily laden 

 with PCB's. White perch fished in the Hudson River 

 appear to be strong candidates for regulatory action. 

 Total PCB content for white perch young-of-a-year 

 (YOY) sampled from the Hudson River was 1.9 ppm. 



Striped bass sampled from estuaries of the Hudson 

 River averaged 1.5 ppm. Range of PCB results from 

 five samples indicate that this species is another can- 

 didate in need of more intensive monitoring. A sam- 

 ple of the YOY had a total PCB content of 1.1 ppm. 

 One sample from the New York Bight Apex had a 

 PCB value of 3.6 ppm. The lowest PCB values for 

 striped bass were found in Lake Mead, Nev. Striped 

 bass fished from Coos River, Oreg., averaged 0.27 

 ppm. Coos River was considered one of the pristine 

 areas for sampling striped bass. Striped bass fished 

 from the San Francisco Delta region averaged 0.39 

 ppm. There is intensive agriculture in the Central 

 Valley of this region with drainage by the Sacramento 

 and San Joaquin Rivers into the Delta and San Fran- 

 cisco Bay. Sites considered to be contaminated from 

 agricultural runoff were sampled. One sample from 

 the Sacramento River had a PCB content of 4.00 

 ppm. Seventy-nine striped bass samples were 

 analyzed from the western coastal U.S. waters. The 

 total PCB content averaged 0.32 ppm. 



Table 3 summarizes PCB values according to fami- 

 ly grouping. The average PCB values in ppm for the 

 following families were: 



porgies 0.07 



sea basses 0.04 



sea chubs 0.02 



scorpionfishes 0.07 



surfperches 0.13 



temperate basses 2.84 



