【摘要】 目的建立测定蛋制品中7种违禁合成性激素的超高效液相色谱-串联质谱(UPLC-MS/MS)分析法。方法样品(咸蛋和皮蛋)经酶解、甲醇提取、ZnCl2去脂、LC-C18和LC-NH2固相柱净化后,以UPLC-MS/MS在正离子化和多反应监测(MRM)模式下进行测定。结果该方法测定蛋制品中醋酸氯地孕酮(Chlormadinoneacetate,CDA)、醋酸甲羟孕酮(Medroxyprogesteroue Acetate,MPA)、醋酸甲地孕酮(Megestrol acetate,MA)、丙酸睾丸酮(Testosterone propionate,TSP)、甲基炔诺酮(Norgestrel,NG)、甲基睾丸酮(Methyltestosterone,MTS)、诺龙(Nandrolone,NT)等7种违禁性激素残留的检测限在(LOD)在0.012~0.23μg/kg范围内,定量限(LOQ)在0.04~0.76μg/kg范围内。在加标水平分别为2μg/kg和4μg/kg时,检测的回收率分别在80.2%~114%和75%~119%的范围内;两种加标水平下,5次平行测定的相对标准偏差分别在6.7%~14.3%和2.9%~7.3%的范围内。结论该法灵敏度高、操作简便,能够满足于禽蛋及蛋制品中违禁性激素多残留监督检测。更多还原

【Abstract】 Objective To develop method of 7 banded synthesis sex hormones residues in egg products determinated by ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.Methods The sample were enzymolied and target compounds were extracted with methanol.ZnCl₂ was added to the extract solution to remove lipid and then analytes were purified by LC-C 18 and LC-NH₂ solid phase extraction cartridge and further determined by UPLC-MS/MS under positive ionization and multiple reaction monitoring（MRM）modes.Results The limits of detection（LOD）of UPLC-MS/MS method used for testing Chlormadione acetate（CDA）,Medroxypogesterone acetate（MPA）,Megestrol Acetate（MA）,Testosterone propionate（TSP）,Norgestrel（NG）,Methyltestosterone（MTS）and Nandrolone（NT）in egg products ranged from 0.012 to 0.23μg/kg,and the limits of quantification（LOQ）were from 0.04 to 0.76μg/kg.Experiments on spiked samples of egg products showed that at addition level of 2.0μg/kg,the average recoveries of the sex hormones ranged from 80.2% to 114%,and coefficients of variation from 6.7% to 14.3%;while at addition level of 4.0μg /kg,the average recoveries ranged from 75% to 119%,and coefficient of variation from 2.9% to 7.3%.Conclusion The method could be able to identify and quantify banded synthesis hormones residues in eggs and egg products.It coubld be simple and sensitive,suitable for statutory residue testing.更多还原