To control and prevent parasites infect poultry and livestock in barn with used carbaryl and permethrin. The domestic animals will exposure long-time in this materials because of cleaning and disinfect. carbaryl (CRB), permethrin (PER) and piperonyl butoxide (PBO) were belong to endocrine disrupters substance, therefor, these materials were have maximum residue limits internationally, but there are no analytical method to detect the residues of CRB,PER and PBO in livestock and poultry products. In order to prevent the problem of CRB, PER and PBO residues in livestock and poultry products, a precise, accurate and rapid analytical method for examining CRB, PER and PBO in livestock and poultry products must be developed. Samples were extracted with acetonitrile; the following cleanup was carried out on a primary secondary amine absorbents. For CRB was detected by high performance liquid chromatography. For PER and PBO was detected by Gas Chromatography-Mass Spectrum. The liner concentration range of the calibration curves of CRB, PER and PBO were 0-500 ng/mL (R2 = 0.9999), 0-60 (R2 = 0.9976) and 0-70 ng/mL (R2 = 0.9984), respectively. The limit of detection (LOD) of CRB, PER and PBO were 5.0, 3.5 and 3.2 ng/mL, respectively and limit of quantification (LOQ) were 16.6, 11.7 and 10.6 ng/mL, respectively. Recoveries of spiking experiments at three different concentration levels of CRB, PER and PBO, 0.2, 1.0 and 2.0 ng/mL in livestock and poultry products samples were 72-112%. The corresponding inter-day and intra-day precision expressed at relative standard deviations (RSD %) were 1.8-9.3% and 1.6-13.3%, respectively. No CRB, PER and PBO residues were detected in the real samples. Overall, the developed method exhibited with rapid analysis, good sensitivity, reproducibility, repeatability, and accuracy for the analysis of CRB, PER and PBO residue in livestock and poultry products.