超高压液相色谱-串级质谱分析渔业水中7种激素药物  

Determination of 7 hormones in fisheries water by ultra high-pressure liquid chromatography coupled tandem mass spectrometry

作　　者：张立坚[1] 王秀季[1] 张良滔[1] 张俊杰[1] 蔡春[1] 

机构地区：[1]广东医学院分析中心,湛江524023

出　　处：《分析试验室》2012年第1期58-62,共5页Chinese Journal of Analysis Laboratory

基　　金：广东省科技计划项目(2009B020316005)资助

摘　　要：建立了同时测定渔业养殖水中氢化可的松、泼尼松、醋酸可的松、睾酮、甲睾酮、黄体酮及苯丙酸诺龙等7种激素残留药物的超高压液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)分析方法。水样用HLB固相萃取柱净化、浓缩后,洗脱液经氮气吹干,残渣用乙腈-水(V:V=1:1)溶解,以乙腈和0.1%甲酸水溶液为流动相,经ZORBAX SB-C18色谱柱分离后进行LC-MS/MS多反应检测模式作定性定量分析。方法在0.5～40μg/L或1～40μg/L范围具有良好的线性,相关系数大于0.997,检出限(S/N=3)为0.03～0.3μg/L,平均回收率为74.8%～113.0%,相对标准偏差为4.0%～16%。方法适用于渔业养殖水中7种激素的检测分析。An ultra high-pressure liquid chromatography coupled electrospray ionization triple-qudruple tandem mass spectrometric（UHPLC-ESI MS/MS） method has been established for the simultaneous determination of 7 hormones,including cortisone acetate,cortisol,nandrolone prednisone,phenylpropionate,progesterone,Methyltestosterone and testosterone,in fisheries water.The hormones were extracted and cleaned up by an Oasis HLB solid phase extraction cartridge.The extract was evaporated to dryness under nitrogen,and reconstituted in acetonitrile-water（1：1,by volume）.The 7 hormones were separated and detected by ZORBAX SB-C18（2.1×50 mm,1.8μm）using 0.1% formic acid（A） and acetonitrile（B） as mobile phase.The target compounds were confirmed and quantified by MS/MS under multiple reaction monitoring（MRM） mode with external standard method.Under the optimal conditions,the calibration curves of 7 hormones showed good linearity with the correlation coefficients 0.997 in the range of 0.5 or 1～40μg/L,the limits of detection（LODs） ranged from 0.03 to 0.3μg/L（S /N = 3）,the average recoveries of 7 hormones were in the range 74.8%～113.0%,the relative standard deviations（RSDs） were 4.0%～16%.

关 键 词：超高压液相色谱-电喷雾电离质谱 激素 固相萃取 渔业用水 

分 类 号：O657.63[理学—分析化学]