摘要
目的:固相萃取高效液相色谱法同时测定水产品中己烯雌酚(DES)、甲基睾酮(MET)的残留量。方法:固相萃取小柱为AlltechExtract cleancolumnsC18,2 0 0mg/ 4.0ml,洗脱液为甲醇;色谱柱为SUPELCODiscoveryC185 μm2 5 0×4.6mm ,流动相为:甲醇∶水=75∶2 5 (V/V) ,流速为1 0ml/min ,二极管阵列检测器,检测波长为2 4 5nm。结果:该方法的线性范围为:0.5～10.0 μg/ml;标准曲线线性良好,其回归方程及相关系数r分别为己烯雌酚:y =6 1 3 10 4 2x+ 2 3 86 15 ,r =0 99994 ;甲基睾酮:y =6 6.5 5 4 2 7x + 2.3 2 4 91 ,r =0.99994。最低检出限分别为:己烯雌酚9 5 μg/kg ;甲基睾酮5 4μg/kg ;回收率在95 %～10 2 %之间,相对标准偏差小于1.3 %。结论:该方法操作简便、快捷。
Objective:To establish a rapid,simple and sensitive SPE high performance liquid chromatographic method for the determination of male and female hormon residues in aquaculture.Method:The SPE column was Alltech Extract-clean columns C18,200 mg/4.0 ml.The elutropic liquid was Methanol.The filtrate was examined by HPLC.Chromatographic column was Discovery C18 5 μm 250×4.6 mm,mobile phase was:Methanol:Water=75∶25(V/V),flowing rate was 1.0 ml/min,DAD detecting wavelength was 245 nm.Results:Regression equation and r:Diethylstilbestrol y=61.31042x+2.38615,r=0.99999;Methyltestosterone y=66.55427x+2.32481,r=0.99994;The method detective limit was 9.5 μg/kg(Diethylstilbestrol),5.4 μg/kg(Methyltestosterone);The recoveries of hormon was 95%～102% and the relative standard deviation was less than 1.3%.Conclusion:The method was proved to be satisfactory in precision,accuracy and sensitivity.
出处
《现代预防医学》
CAS
北大核心
2005年第4期287-289,共3页
Modern Preventive Medicine
基金
广东省医学科学技术研究基金项目 (A2 0 0 45 85 )
