液相色谱-串联质谱法测定谷物类饲料中的41种激素  

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

作　　者：张毅[1] 蓝芳[1] 张峰[2] 沈金灿[1] 储晓刚[2] 

机构地区：[1]深圳出入境检验检疫局,广东深圳518045 [2]中国检验检疫科学研究院,北京100023

出　　处：《色谱》2011年第6期523-534,共12页Chinese Journal of Chromatography

基　　金：国家质检总局科技计划项目(2008IK167)

摘　　要：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,3.0μm)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5.0～200.0μg/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0.123～2.72μg/kg。在5、40、200μg/kg或10、40、200μg/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。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 μg/kg with the correlation coefficients above 0.99 and the limits of quantification（LOQs,S/N≥10） were 0.123-2.72 μg/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.

关 键 词：液相色谱-串联质谱 雄性激素 孕激素 糖皮质激素 雌性激素 二羟基苯甲酸内酯 谷物类饲料 

分 类 号：O658[理学—分析化学]