Simultaneous Determination of Methyltestosterone and Diethylstilbestrol in Aquatic Products by Gel Permeation Chromatography-High Performance Liquid Chromatography

KeyWord:gel permeation chromatography£¨GPC)  solid phase extraction£¨SPE)  high performance liquid chromatography£¨HPLC)  aquatic products  methyltestosterone£¨MET)  diethylstilbestrol£¨DES)

Abstract:

      A method of high performance liquid chromatography combined with gel permeation chromatography£¨GPC/HPLC) was developed for the simultaneous analysis of methyltestosterone£¨MET)and diethylstilbestrol£¨DES) in aquatic products.The homogenized samples were extracted with diethyl ether,then cleaned by GPC using ethyl acetate-cyclohexane£¨1¡Ã1)as mobile phase,follwed by a further HLB solid phase extraction.The targeted compounds were detected by HPLC-ultraviolet detector at the wavelength of 254 nm,using methanol-water£¨72¡Ã28) as mobile phase,and quantified by the external standard method.The calibration curves of two compounds were linear in the concentration range of 0.02-2.0 mg/L with correlation coefficients more than 0.999.The average recoveries of MET and DES at spiked concentrations of 10.0,50.0,200 ¦Ìg/kg ranged from 84% to 93%,with relative standard deviations£¨RSDs) less than 6.0%.The LOQs of MET and DES were 6.0 ¦Ìg/kg and 5.0 ¦Ìg/kg,respectively.