Abstract: Total thiol and reduced glutathione in Kiwi, Jujube and Fruit Physalis had been determined by UV-vis spectrometry and fluorescent spectrometry using 5, 5-dithio-bis-nitrobenzoic acid (DTNB) and O-phthaldehde (OPA) as derivatizing agents. Relative amount between total thiol and GSH varies significantly, among which kiwi and jujube contained relative large amount of GSH with the content of 0.7092, 0.8374mol/g respectively, while fruit physalis contained higher amount of total thiol with the centent of 1.4173mol/g. The determination of total thiol and GSH proceeded with the accurate and sensitive method with the recovery range of 95.38%～101.9% , and lowest detection limits reached to 9.6×10 -7 , 2.69×10 -7 mol/L respectively.