液相色谱-串联质谱法测定动物组织中1，2-二苯乙烯类药物残留的研究

建立了固相萃取-液相色谱-串联质谱法同时测定动物组织中3种1,2-二苯乙烯类药物（包括己二烯雌酚、己烯雌酚、己烷雌酚）残留量的方法。试样中的药物经甲醇超声提取后，过HLB固相萃取柱净化、氮吹至干，用流动相溶解后进行液相色谱 串联质谱法测定，以D₈-己烯雌酚为内标进行定量分析。方法的最低检出限为0.2 μg?kg^-1，定量限均为0.5 μg?kg^-1；在1.0～100 μg?L^-1 范围内线性良好；加标浓度在0.5～10 μg?kg^-1 范围内，动物组织中己二烯雌酚、己烯雌酚、己烷雌酚的回收率在78.8％～110.9％，批内相对标准偏差小于或等于8.0％，能满足相关法规要求。

Determination of 1,2-Stilbenes Residues in Animal Tissues by Liquid Chromatography-Tandem Mass Spectrometry

A new solid phase extraction-liquid chromatography-tandem mass spectrometry（SPE-LC-MS/MS）method for simultaneous determination of 1,2-stilbenes, diethylstilbestrol (DES), dienoestrol (DIS) and hexestrol (HES) in animal tissues was reported. The 1,2-stilbenes were extracted with methanol from analyte by ultrasonic. The extraction was evaporated (40 ℃) to 5 mL, purified by passing through HLB（20 g?L^-1）solid phase extraction cartridges. The elution was evaporated by nitrogen blow and dissolved by mobile phase, and then assayed by liquid chromatography-electrospray ionization tandem mass spectrometry. The limits of detection(LOD) are 0.2 μg?kg^-1, and the limits of quantitation(LOQ) are 0.5 μg?kg^-1. The calibration curves are linear between 1.0 μg?L^-1 and 100 μg?L^-1 for 1,2-stilbenes. Recoveries of DES, DIS, HES in animal tissues are 78.8％～110.9％, and inter-relative standard deviation（n=5）are less than 8.0%, respectively, at spiked levels of 0.5～20 μg?kg^-1. The method is simple, sensitive and reliable for food safety.