Several analytical methods were developed to determine cypermethrin and its acid metabolite residues in bovine milk, cream, kidney, liver, muscle, and fat samples. These methods used solvent extraction or acid reflux, liquid-liquid and/or solid phase extraction, with or without chemical derivatization, and quantitation by gas chromatograph with electron capture or mass selective detector. The LOQ and LOD for milk were set at 10 and 2 ppb, respectively. The average method recoveries for cypermethrin, cis-DCVA, trans-DCVA, and m-PBA in cow milk were 81% (n=39), 96% (n=22), 99% (n=22), and 106% (n=22), respectively. For bovine tissues and cream samples, the LOQ and LOD were 50 and 10 ppb, respectively. The overall average method recoveries for cypermethrin, cis-DCVA, trans-DCVA, and m-PBA in cream and tissue samples were 92% (n=27), 97% (n=25), 103% (n=25), and 98% (n=25), respectively. Satisfactory recoveries were also obtained with higher fortification levels for milk and fat samples.