【摘要】 建立了动物组织中己烯雌酚(DE S)、己二烯雌酚(D IS)和己烷雌酚(H S)残留量的气相色谱-质谱分析方法。动物组织样品在碱性条件下用乙酸乙酯提取,经碳酸钠溶液液-液分配净化,再用硅胶柱固相萃取净化,洗脱液均分成两份后经氮气吹干,分别用双三甲基硅基三氟乙酰氨(B STFA)和七氟丁酸酐(HFBA)衍生,采用选择离子监测模式(S IM)进行测定,外标法定量。检出限为0.30μg/kg(cis-DE S),0.10μg/kg(tran s-DE S和H S)和0.15μg/kg(D IS)。在0.5~4.0μg/kg添加水平,回收率为73.0%~86.5%,相对标准偏差(RSD)为1.0%~7.2%。衍生物的峰面积与样品浓度在10~1 000μg/L(DE S和D IS)和5~500μg/L(H S)范围内呈良好的线性关系,线性回归系数大于0.99。更多还原

【Abstract】 A method has been developed to determine residual stilbenes such as diethylstilbestrol(DES),dienestrol(DIS) and hexestrol(HS) in animal tissues using solid phase extraction(SPE) and gas chromatography-mass spectrometry(GC-MS).The procedures for extraction,cleanup on an LC-Si solid phase extraction cartridge and derivatization of stilbenes were established and optimized.The analytes were detected by mass spectrometer with electron impact source in selected ion monitoring mode(EI/SIM),and quantified with an external standard calibration curve method.Linear calibration curves were obtained in the concentration ranges from 5 to 500 μg/L for HS and from 10 to 1 000 μg/L for DES and DIS(the correlation coefficients were above 0.99).Recoveries of the stilbenes were 73.0%-86.5%,and the relative standard deviations were between 1.0% and 7.2%.The limits of detection were 0.30 μg/kg for cis-DES,0.10 μg/kg for trans-DES and HS and 0.15 μg/kg for DIS in pork and swine liver.更多还原