GC-MS法测定肉中雌激素残留量方法的研究

Analysis of estrogen residue in meat utilizing GC-MS

目的:建立GC-MS法测定肉中雌二醇、戊酸雌二醇、炔雌醚、苯甲酸雌二醇残留量的方法。方法:样品经乙腈超声萃取、离心,提取液经二氯甲烷反萃取、浓缩至干,残留物经交联葡聚糖LH-20柱净化后作TMS化反应,用GC-MS的SIM方法测定。结果:4种组分分离良好,并得到浓度与峰面积成正比的工作曲线,相关系数r>0.997;其变异系数CV≤1.2%(n=6),最低检出限≤20 ng/g,回收率范围为84.6%～92.4%。结论:该法具有灵敏、准确、精密、无杂质干扰等优点。

Objective：To study a method for the determination of Estradiol, Estradiol valerate, Quinestrol, Estradiol benzoate residue in meat by GC - MS. Methods： The 4 kinds of components were extracted from homogenized samples with methanol and dichloromethane, followed by solid - phase extn. with LH - 20 column, and trimethylsilylation at 600C for 30 min, then the GC - MS method in selected ion monitoring mode （SIM） was used to analyze them. Results： Good separation was achieved in the 4 components and the standard curve showing a direct ratio between the concentration and the peak area was obtained, r 〉 0. 997, CV≤1.2% （n = 6） ; the detection limits were below 20 ng/g ; The recovery was between 84. 6% and 92.4%. Conclusion： The method is satisfactory in precision, sccuracy and sensitivity.