动物组织中多种残留非类固醇同化激素的液相色谱-串联质谱法同时测定

Simultaneous Determination of Residual Nonsteroid Anabolic Hormones in Animal Tissues by Liquid Chromatography-Tandem Mass Spectrometry

用液相色谱-串联质谱（LC—MS／MS）同时测定动物组织中玉米赤霉醇（ZER）、玉米赤霉酮（ZEAR）、已烯雌酚（DES）、已烷雌酚（HEX）、双烯雌酚（DEN）。动物组织均质后，用叔丁基甲基醚和乙酸盐缓冲液加酶解剂分别提取试样中残留激素及代谢物，经硅胶柱净化，应用LC—MS／MS大气压化学电离负方式（APCI-），以多反应离子监测（MRM）方式进行检测，方法检测能力（CCβ）为0、143～0．496ng·g^-1。选用ZER、DES的同位素标记物作内标，内标法定量。DES、DEN在0．5-10ng·g^-1范围内回收率为58％～108％，ZER＋TAL、ZEAR、HEX在0．25—5ng·g^-1范围内回收率为66％-109％。

A liquid chromatographic （ LC ） - tandem mass spectrometry （MS/MS） method was developed for simultaneous determination of zeranol （ ZER）, zearalanone （ ZEAR）, diethylstilbestrol （ DES）, hexestrol（HEX）, and dienoestrol （DEN） in animal tissue samples. The analytes were extracted with methyl tert-butyl ether and acetate buffer solution from the tissues after homogenization. The extract was cleaned up with a silica gel column before analysis. Detection capabilities（CCI3） related to the transition products of lowest abundance for the method were 0. 143 -0. 496 ng · g^-1 in tissue and were achieved using atmospheric pressure chemical ionization（APCI） in negative ion scan and multiple reaction monitoring（MRM） determination modes. Isotopically-labeled ZER-d4 and DES-d8 were used as internal standard in this method. The recoveries of the method were 58% - 108% for DES and DEN between 0. 5 and 10 ng·g^-1, and 66% - 109% for ZER, ZEAR and HEX between 0. 25 and 5 ng · g^-1 respectively.