建立了液相色谱-串联质谱(LC-MS/MS)测定尿液中的内源性类固醇激素的方法.尿样经葡萄糖醛酸甙酶酶解后进行液-液提取,以甲醇-0.1%甲酸缓冲液(含0.02 mol/L乙酸铵)(体积比为68∶32)为流动相,采用Cosmosil C18色谱柱分离,并以三重四极杆串联质谱多反应监测扫描方式对尿样中的脱氢表雄酮(DHEA)、睾酮、表睾酮、雄酮和苯胆烷醇酮等5种激素进行检测.方法的最低检出限为0.01～10 ng/mL,平均回收率为96.7%～106.5%,日内和日间相对标准偏差(RSD)分别小于7%和11%.应用所建立的方法测定了健康志愿者口服DHEA后尿液中内源性类固醇激素的变化情况,结果表明该方法样品处理简便,色谱分离完全,结果准确可靠,可替代气相色谱-质谱法用于体液中内源性类固醇激素兴奋剂的常规分析.
参考文献
| [1] | Lu C Y.Conspectus on doping in sport.Shanghai:Shanghai Scientific and Technical Literature Press(卢昌亚.运动兴奋剂概论.上海:上海科学技术出版社),1999:101 |
| [2] | Corrigan B.Clin J Sport Med,2002,12:236 |
| [3] | Labrie F,Luu-The V,Bélange A et al.J Endocrinol,2005,87:169 |
| [4] | Dehennin L,Ferry M,Lafarge P,et al.Steroids 1998,63:80 |
| [5] | WADA Project Team.Reporting and evaluation guidance for testosterone,epitestosterone,T/E ratio and other endogenous steroids.http://www.wada-ama.org/rtecontent/document/end_steroids_aug _ 04.pdf |
| [6] | Daeseleire E,Vandeputte R,Van Peteghem C.Analyst,1998,123:2 595 |
| [7] | Kintz P,Cirimele V,Sachs H et al.Forensic Sci Int,1999,101:209 |
| [8] | Griffiths W J,Liu S,Alvelius G,et al.Rapid Commun Mass Spectrom,2003,17:924 |
| [9] | Yvan G.J Chromatogr B,1999,735:189 |
| [10] | Baulieu E E,Robel P.Proc Natl Acad Sci USA,1998,95:4 089 |
| [11] | Thieme D,Sachs H.Anal Chim Acta,2003,492:171 |
| [12] | Van Poucke C,van de Velde M,Van Peteghem C.J Mass Spectrom,2005,40:731 |
| [13] | Choi M H,Kim K R,Chung B C,2000,65:54 |
| [14] | Guan F,Uboh C E,Soma L R,et al.J Chromatogr B,2005,829:56 |
| [15] | WADA Project Team.Minimum required performance limits for detection of prohibited substance.(2004-01-15).http://www.wada-ama.org/rtecontent/document/perflimits2.pdf |
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