建立了能够同时检测牛肉组织中玉米赤霉醇(又名α-玉米赤霉醇)及3种相关物(β-玉米赤霉醇、玉米赤霉酮和α-玉米赤霉烯醇)残留的气相色谱-质谱联用法。样品均质后,用甲醇提取样品中的待测物,浓缩,用水稀释后,乙酸乙酯萃取,浓缩。用氢氧化钾溶液溶解,正己烷去脂,乙醚萃取,氨基固相萃取柱净化,衍生化后,用气相色谱-质谱联用仪检测,外标法定量。玉米赤霉醇、β-玉米赤霉醇、玉米赤霉酮和α-玉米赤霉烯醇线性范围均为0.5-10.0 ng/mL,检测限均为1.0 ng/g,在添加5.0 ng/g时,回收率为71.5%-81.4%,变异系数为1.4%-5.0%。
A method for determination of zeranol and related compounds(talernol, zearalanone, α-zearalenol)in bovine muscle by gas chromatography-mass spectrometry was described. The samples were extracted with methanol, condensed, diluted with water and extracted with ethyl acetate. Then hexane was added to remove the fat. The solution was extracted with KOH and then with a ether, cleaned up with NH2-SPE. After derivatization, the samples were analysed by gas chromatography-mass spectrometry. The linear range was 0. 5-10. 0ng/mL and the limit of detection was 1.0 ng/g. Recoveries were 71.5%-81.4% with CVs of 1.4%-5.0% at spiked levels of 5.0 ng/g.