Abstract: The synthesis of ¹¹C-acetate and ¹⁸F-acetate was carried out by CFN-MPS200 multi-functional synthesizer, and the quality control comparison analysis was obtianed by TLC method and HPLC method. ¹¹CO₂ was released into 1.0 mol/L methylmagnesium bromide in THF solution. After 2 min, it was hydrolyzed with 1 mol/L hydrochloric acid. The reaction solution was purified by ON Grad-Ag and ON Grad-H column, and then adsorbed by PS-OH column. The saline was rinsed, and finally purified by a CM column and filtered through a sterile filter to obtain ¹¹C-acetate. The synthesis time was about 10 min, and the EOS%=(53.5±5)%（n=6）. Substitution reaction of ¹⁸F^- with benzyl bromide, the impurities were removed by adsorption on a C-18 column, eluted by alkali hydrolysis, purified by IC-H, PS-2, alumina column and subjected to sterile filtration to obtain product ¹⁸F^- Acetate. The synthesis time was 40 min, and the EOS%=（20.2±5）%（n=5）. The TLC and HPLC quality control analysis of the two types of acetate compounds were carried out. The 95% (V∶V) acetonitrile aqueous solution was used as the developing agent of TLC, the R_f values were 0.31 min and 0.60 min, respectively, and the radiochemical purity was more than 99%. With HPLC injection quality control, the peak time of the UV detector and the radioactivity detector is between 2.3-2.4 min, and the chemical purity and radiochemical purity are greater than 99%.The synthesis of ¹¹C-Acetate and ¹⁸F-Acetate is automatically synthesized by CFN-MPS200 synthesizer, without human intervention, the synthesis process is simple, the synthesis yield is stable. Radiochemical purity and chemical purity are high, which can meet the clinical requirements.