同位素稀释液相色谱串联质谱法同时测定饲料中雌激素类药物

发布时间：2018-11-10 16:04

【摘要】：试验旨在建立饲料中8种雌激素类药物的同位素稀释液相色谱串联质谱分析方法。样品用乙腈提取,提取液经氮吹后用乙酸乙酯复溶,再利用碳酸钠溶液进行液液萃取净化,净化后吹干乙酸乙酯层,用40%乙腈溶液溶解残渣,经离心过滤膜后进行液相色谱串联质谱分析。采用Acquity HSS T3色谱柱分离,用水-乙腈作为流动相进行梯度洗脱,电喷雾负离子模式电离,多反应监测模式检测,同位素稀释内标法定量。结果表明:8种雌激素类药物在1.0~200μg/L范围内线性良好,相关系数均在0.9910~0.9992;在1.0~50.0μg/kg添加水平范围内,平均添加回收率在97.5%~106%。本方法中8种雌激素类药物在饲料中的检测限为0.15~0.30μg/kg,定量限为0.50~1.0μg/kg。该方法能满足饲料中8种雌激素类药物含量分析的要求。
[Abstract]:The aim of this study was to establish an isotope dilution liquid chromatography-tandem mass spectrometry method for the determination of eight estrogens in feed. The sample was extracted by acetonitrile, then dissolved by ethyl acetate after nitrogen blowing, then purified by sodium carbonate solution. After purification, the layer of ethyl acetate was dried, and the residue was dissolved with 40% acetonitrile solution. Liquid chromatographic tandem mass spectrometry (LC-MS) was used after centrifuge filtration membrane. Acquity HSS T3 column was used for separation, water-acetonitrile was used as mobile phase for gradient elution, electrospray anion mode ionization, multi-reaction monitoring mode detection, isotope dilution internal standard method. The results showed that the linear range of the eight estrogens was 1.0 渭 g / L, the correlation coefficient was 0.9910 ~ 0.9992, and the average recovery was 97.5m ~ (106) in the range of 1.0 ~ 50.0 渭 g/kg. The detection limit of 8 estrogens in feed was 0.15 ~ 0.30 渭 g 路kg ~ (-1) and the quantitative limit was 0.50 ~ 1.0 渭 g 路kg ~ (-1) 路kg ~ (-1). This method can meet the requirement of 8 estrogens in feed.
【作者单位】：中国动物疫病预防控制中心;宁波市农业科学研究院;
【基金】：宁波市农业科技攻关项目(2013C11003、2015C50067)
【分类号】：O657.63;S816.17

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