Stan H J, Abraham B
J Chromatogr. 1980 Jul 18;195(2):231-41. doi: 10.1016/s0021-9673(00)96814-6.
The residues in meat of seven estrogenic drugs used in anabolic preparations for animal production were analysed as trimethylsilyl ethers by electron-impact gas chromatography-mass spectrometry following a simple clean-up procedure. The compounds under investigation were: 17 beta-estradiol,l diethylstilbestrol,l hexestrol, dienestrol, stilbestrol, ethynylestradiol and zeranol. The method includes extractive homogenization of 10 g of meat in tetrahydrofuran, followed by liquid-liquid partition between acetonitrile and hexane and finally a chromatographic purification step on a small silica gel column. Gas chromatography was carried out on a 10-m glass capillary column coated with SE-54 using a temperature program from 100 to 250 degrees C. The capillary column was connected to the ion source by an all-glass open-split interface with a scavenger gas-line. Detection of anabolic residues was performed with selected ion monitoring on intensive ions in the mass region above m/e 400, resulting in a detection limit of 1-5 ppb (10(9)). Quantitative determinations were performed using dodecyl gallate as an internal standard applying the signal ratio of the drug and the standard.
采用简单的净化程序后，通过电子轰击气相色谱 - 质谱联用仪，将动物生产用合成代谢制剂中使用的七种雌激素药物在肉中的残留分析为三甲基硅醚。所研究的化合物为：17β - 雌二醇、己烯雌酚、己烷雌酚、双烯雌酚、己烯雌酚、乙炔雌二醇和玉米赤霉醇。该方法包括在四氢呋喃中对10克肉进行萃取均质，然后在乙腈和己烷之间进行液 - 液分配，最后在小型硅胶柱上进行色谱纯化步骤。气相色谱在涂有SE - 54的10米玻璃毛细管柱上进行，采用100至250℃的温度程序。毛细管柱通过带有清除气体管线的全玻璃开口分流接口连接到离子源。通过对m/e 400以上质量区域的强离子进行选择离子监测来检测合成代谢残留，检测限为1 - 5 ppb（10⁻⁹）。使用没食子酸十二酯作为内标，应用药物与标准品的信号比进行定量测定。
