【摘要】 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0.2μg.kg-1,定量限均为0.5μg.kg-1;在1.0~100μg.L-1范围内线性良好;加标浓度在0.5~10μg.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。更多还原

【Abstract】 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.更多还原