A rapid method was developed for the extraction, isolation, and detection of polybrominated biphenyls (PBBs) from plasma, feces, milk, and bile, using disposable glassware. Use of disposable equipment greatly reduced the amount of laboratory background and cross-contamination of samples. The procedure employed a multiple extraction with a mixture of diethyl and petroleum ethers, followed by cleanup on miniature Florisil, silica gel, and sodium sulfate columns. Detection was accomplished by gas chromatography. Recoveries were determined for the six major components of a commercial PBB mixture and were approximately 96% for plasma, 59% for feces, and 98% for milk. The background levels for plasma, feces, and milk were 0.0005, 0.0007, and 0.0007 ppm, respectively, bringing the minimum detectable limits of the major hexabromobiphenyl peak to 0.0010, 0.0014, and 0.0014 ppm on a whole tissue basis.