摘要
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(ZnCl2)去脂、LC-C18和LC-NH2固相萃取柱净化、WatersAC-QUITYTMUPLCBEH-C18色谱柱(100mm×2.1mm,1.7μm)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0.08～0.17μg/kg,定量限(S/N=10)为0.24～0.58μg/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1,4μg/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.ZnCl2 was added to the extract solution to remove lipids.Then target compounds were purified by an LC-C18 and an LC-NH2 solid phase extraction cartridges.The target compounds were separated on a Waters ACQUITYTM UPLC BEH-C18 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.
出处
《色谱》
CAS
CSCD
北大核心
2010年第2期190-196,共7页
Chinese Journal of Chromatography
基金
浙江省质检系统重大科研计划项目(20070106)
关键词
超高效液相色谱-串联质谱法
性激素
多残留
鱼制品
ZnCl2去脂
ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-MS/MS）
sex hormones
multi-residues
fish products
ZnCl2 delipidation
