A method was established for the separation and determination of diethylstilbestrol and four sedatives (estazolam, alprazolam, chlordiazepoxide and diazepam) in pig blood tofu by modified solid-phase dispersive extraction with high performance liquid chromatography. The anhydrous sodium sulfate and florisil(the ratio of quality 4:1)was the dispersing agent and clean-up reagent in the process of modified solid-phase dispersive extraction. The methanol was chose as the solvent .The estrogen and sedatives were separated on C18 column (5 μm, 250 mm × 4.6 mm i.d.)employing methanol:acetonitrile:water=30:30:40 as mobile phase and deter-mined using UV detector at 235 nm. The column temperature was 30 ℃.The flow rate of mobile phase was 1.0 mL/min. The linearity was good in the range of 0.010μg/mL-10μg/mL with the correlation coefficients above than 0. 9992. The limit of detection of sedatives was 10 ng/g and the limit of detection of diethylstilbestrol was 15 ng/g The average recoveries of estrogen were 82.4%to 104.5%. The relative standard deviations were 1.7%-3.5%. The method is simple, quick and inexpensive, which was available for the detection of diethyl-stilbestrol and sedatives in pig blood tofu.%建立改进了的基质固相分散萃取(MSPD)-高效液相色谱法(HPLC/UVD)同时快速检测猪血豆腐中的4种镇静剂(艾司唑仑、阿普唑仑、氯氮和地西泮)及己烯雌酚残留的方法.样品以无水硫酸钠和弗洛里西土(质量比4:1)为分散剂和净化剂,甲醇为溶剂.色谱条件:C18色谱柱(5μm,250 mm×4.6 mm i.d.),甲醇-乙腈-水(体积比30:30:40)为流动相,流速:1.0 mL/min,检测波长235 nm,柱温:30℃.5组分在0.010μg/mL~10μg/mL范围内线性关系良好,相关系数均不低于0.9992.猪血豆腐中4种镇静剂的方法检出限均为10 ng/g,己烯雌酚的方法检出限为15 ng/g;5组分平均回收率在82.4%~104.5%之间,相对标准偏差为1.7%~3.5%.结果表明该方法简便、快速、经济,适用于猪血豆腐中己烯雌酚及多种镇静剂类药物残留的快速检测.
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