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以电喷雾离子源(ESI)为电离源,在正离子采集模式下建立了鱼制品中7种性激素(甲基炔诺酮、甲基睾酮、丙酸睾酮、醋酸甲羟孕酮、醋酸甲地孕酮、醋酸氯地孕酮、诺龙)的超高效液相色谱-质谱/质谱(UPLC-MS/MS)检测方法.样品被酶解后用甲醇提取,提取液经氯化锌(ZnCl_2)去脂、LC-C_(18)和LC-NH_2固相萃取柱净化、Waters ACQUITY~(TM) UPLC BEH-C_(18)色谱柱(100 mm×2.1 mm,1.7 μm)分离,在多反应监测模式下进行UPLC-MS/MS分析.7种性激素的方法检出限(S/N=3)为0.08～0.17 μg/kg,定量限(S/N=10)为0.24～0.58 μg/kg.考察了内标法和基质匹配外标法对7种性激素进行定量的回收率与精密度:添加水平为1,4 μg/kg 时,以内标法定量,7种性激素的平均回收率为76% ～118% ,相对标准偏差(RSD)为5.0% ～11.3% ;以基质匹配外标法定量,7种性激素的平均回收率为66% ～94% ,RSD为4.5% ～10.7% .该结果表明两种方法均能够满足鱼制品中7种性激素的多残留检测要求.应用建立的方法对市售脱脂大黄鱼及烤鱼片进行检测,未发现7种目标违禁性激素.

A rapid,specific and highly sensitive method for the determination of seven sex hormones (norgestrel,methyltestosterone,testosterone propionate,medroxyprogesterone acetate,megestrol acetate,chlormadinone acetate,and nandrolone) residues in fish products was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization (ESI) in positive mode.The target compounds were extracted with methanol after the enzyme hydrolysis of the fish products.ZnCl_2 was added to the extract solution to remove lipids.Then target compounds were purified by an LC-C_(18) and an LC-NH_2 solid phase extraction cartridges.The target compounds were separated on a Waters ACQUITY~(TM) UPLC BEH-C_(18) column (100 mm×2.1 mm,1.7 μm) and detected qualitatively and quantitatively in multi reaction monitoring (MRM) mode.For the seven sex hormones,the limits of detection (LOD) of the method were from 0.08 to 0.17 μg/kg and the limits of quantification (LOQ) were in the range of 0.24-0.58 μg/kg.At the spiked levels of 1 and 4 μg/kg,the average recoveries ranged from 76% to 118% with the relative standard deviations between 5.0% and 11.3% for the seven sex hormones using internal standard method; and the average recoveries ranged from 66% to 94% with the relative standard deviations between 4.5% and 10.7% using matrix matched external standard method.The results showed that both methods are able to meet the multi-residue detection of the seven sex hormone residues in fish products.The degreased large yellow croaker and roast fish fillet real samples from a local market were detected by the developed method,and the seven targets were not found.