硅胶柱SPE-HPLC测定水产品中甲基睾酮的研究

Silica gel column SPE-HPLC determination of methyltestosterone in aquatic products

建立了硅胶柱固相萃取高效液相色谱法测定水产品中甲基睾酮残留量的方法。固相萃取柱为硅胶柱,洗脱液为丙酮-正己烷(60+40);色谱柱为ZORBAX SB-C184.6mm×250mm5-Micron;流动相为乙腈∶水=58∶42,流速为1.0mL/min;紫外可变波长检测器,检测波长为245nm。结果表明,方法线性范围为0.05～10μg/mL;标准曲线线性关系良好,回归方程和相关系数分别为y=67.43543x-0.0554718,r=0.99998;方法最低检出限为10μg/kg;样品加标回收率在85.2%～94.6%之间,相对标准偏差小于3.5%。该方法检测水产品中甲基睾酮残留量快速、准确,可作为目前水产品中甲基睾酮残留量检测的合适方法。

Found an appropriate method to determine methyltestosterone of aquatic products. Method： The SPE column was silica gel column, 500 mg/6 mL.The elutropic liquid was acetone and n-hexane （60＋40）. The chromatographic column was ZORBAX SB-C18 4.6 min×250 mm 5-Micron, mobile phase was： acetonitrile： water=58：42, flowing rate was 1.0 mL/min, VWD detecting wavelength was 254 nm. Results： The linearity range of method was 0.05-10 μg/mL.Regression equation and r：y=67.43543x-0.0554718, r=0.99998. The method minimum detectability was 10.0μg/kg. The recoveries of hormone was 85.2%-94.6% and the relative standard deviation was less than 3.5% . Conclusion： The method was good to determined the methyltestosterone of aquatic products