液相色谱-串联质谱法测定谷物类饲料中的41种激素

建立了谷物类饲料中10种雄性激素、11种孕激素、10种糖皮质激素、5种雌性激素以及5种二羟基苯甲酸内酯类药物的液相色谱-串联质谱(LC-MS/MS)检测方法。均质样品经乙酸乙酯提取,以改良的QuEChERS吸附剂分散于提取液中实现快速净化。采用C18色谱柱(150 mm×2.1 mm, 3.0 μm)分离,分别在正、负电喷雾串联质谱多反应监测模式下检测。在优化条件下,41种化合物在5.0～200.0 μg/kg含量范围内有良好的线性相关性,相关系数均不低于0.99,定量限(S/N≥10)为0.123～2.72 μg/kg。在5、40、200 μg/kg或10、40、200 μg/kg 3个添加水平下,豆粕类饲料中各化合物的回收率为70.3%～118.1%,相对标准偏差(RSD)为0.82%～19.5%;玉米类饲料中各化合物的回收率为76.1%～122.8%, RSD为1.3%～15.0%。该方法简便、快速、准确,可用于谷物类饲料中雄性激素、孕激素、糖皮质激素、雌性激素以及二羟基苯甲酸内酯类激素的筛查和测定。

Determination of 41 hormones in cereal feeds by liquid chromatography-tandem mass spectrometry

A method was developed for the determination of 10 androgens, 11 progesterones, 10 glucocorticoids, 5 estrogens and 5 resorcylic acid lactones in cereal feeds by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Ethyl acetate was used to extract the sample, and the mixed QuEChERS sorbents were dispersed for purification. The extract was separated by a C18 column and detected in positive or negative multiple reaction monitoring (MRM) mode. With the optimal conditions, the linear ranges of 41 hormones were 5.0 - 200.0 microg/kg with the correlation coefficients above 0.99 and the limits of quantification (LOQs, S/N > or = 10) were 0.123- 2.72 microg/kg. The method validation was carried out at three spiking levels, and the recoveries were 70.3% - 118.1% for soybean meals with the relative standard deviations (RSDs) of 0.82% - 19.5%, and 76.1% - 122.8% for corn meals with the RSD of 1.3% - 15.0%. This method is simple, fast and credible, can be applied to simultaneous screening and determination of estrogens, progesterones, androgens, glucocorticoids and resorcylic acid lactones belonging to the illegal additive of hormones in cereal feeds.