Determination of residues of anabolic drugs in meat by gas chromatography-mass spectrometry.
Determination of residues of anabolic drugs in meat by gas chromatography-mass spectrometry.
复制标题
气相色谱-质谱法测定肉类中合成代谢药物的残留量。
DOI：
10.1016/s0021-9673(00)96814-6
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发表时间：
1980
影响因子：
4.1
通讯作者：
Bernd Abraham
中科院分区：
文献类型：
--
作者：
H. Stan;Bernd Abraham
采用电子轰击气相色谱-质谱法，通过简单的净化步骤，对动物生产合成制剂中的7种雌激素类药物的三甲基硅醚残留量进行了分析。所研究的化合物为：17β-雌二醇、己烯雌酚、己雌酚、双烯雌酚、己烯雌酚、乙炔雌二醇和玉米赤霉醇。该方法包括将10g肉类在四氢呋喃中提取均质，然后在乙腈和正己烷之间进行液-液分配，最后在小硅胶柱上进行层析纯化。色谱柱为SE-54涂层10 m玻璃毛细管柱，程序升温至100~250℃，通过全玻璃开口接口与离子源连接。合成代谢残留物的检测是通过选择离子监测质量区域上面的密集离子进行的，导致检测下限为1-5 ppb(109)。以没食子酸十二酯为内标，利用药物与标准品的信号比进行定量测定。
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: 17β-estradiol, diethylstilbestrol, 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°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 abovem/e400, resulting in a detection limit of 1–5 ppb (109). Quantitative determinations were performed using dodecyl gallate as an internal standard applying the signal ratio of the drug and the standard.