中文摘要：

利用亚临界1，1，1，2-四氟乙烷（R134a）萃取技术，建立了鱼肉中6种性激素残留的气相色谱-质谱（GC—MS）分析方法。样品中的药物经过亚临界R134a萃取后，先进行冷冻过滤去脂，然后通过C18和NH2固相萃取小柱净化，最后经七氟丁酸酐衍生后，采用GC—MS进行定性与定量分析。本实验确定了亚临界R134a萃取6种性激素的最佳条件为：萃取压力4MPa，萃取温度30℃，夹带剂用量6mL。在此条件下，6种性激素在5～1000μg/L浓度范围内线性关系良好，相关系数均大于0．99；检出限为0．2～1μg/kg（S／N=3）。在3种浓度添加水平（1，5和10μg/b）下，6种激素的平均回收率为70．5％～103．6％，相对标准偏差（RSD）为2．1％～12．5％。采用本方法进行实际样品检测时，在一份罗非鱼样品中检出己烯雌酚残留，残留量为14．6μg／kg。

英文摘要：

A new sample pretreatment method was developed for the determination of six sex hormones in fish using subcritical 1, 1, 1,2-tetrafluoroethane （R134a） extraction coupled with gas chromatogq-aphy-mass spectrometry（GC-MS）. After the extraction process was finished, the fatty co-extracted interference of the sample were removed by freezing filtration. Then the analytes were cleaned up by C~8 and NH2 solid phase extraction. At last, the hormones were derivatived by heptafluorobutyric anhydride （HFBA） followed by GC- MS validation. The optimal extraction conditions for the six sex hormones were as follows： extraction pressure 4 MPa; extraction temperature 40 ℃ and extraction entrainer amount 6 mL. Under these conditions, the calibration curves showed good linearity with correlation coefficients larger than 0. 99 in the hormones concentrations of 5-1000 μg/L; the detection limits were 0.2-1.0 μg/kg （S/N= 3）. At the spiked level of 1, 5 and 10 μg/kg, the mean recoveries were between 70. 5% and 103.6%, and the relative standard deviations （RSDs） ranged from 2. 1% to 12.5%. Finally, the diethylstilbestrol was detected in tilapia samples using the proposed method, and the residue content of which is 14.6 μg/kg.