摘要
建立了同时测定24种性激素的高效液相色谱串联质谱法,包括:睾酮、甲基睾酮、诺龙、苯丙酸诺龙、群勃龙、康力龙、勃地酮、雄烯二酮、美雄酮、炔诺酮、乙酸甲孕酮、乙酸甲羟孕酮、乙酸氯地孕酮、17α羟基孕酮、21α羟基孕酮、甲羟孕酮、左炔诺孕酮、雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、己烯雌酚、双烯雌酚。乙酸乙酯提取2次,硅胶柱净化。采用甲醇、水作为流动相,经过CAPCELLPAK C18色谱柱分离后,采用APCI离子源,外标法定量。方法定量限为0.5～2μg/kg,加标回收率为80%～102%,相对标准偏差为6%～10%。方法实现了3类性激素的同时定量及确证分析。
A high performance liquid chromatography-atmospheric-pressure chemical ionization triple-quadruple tandem mass spectrometric（HPLC-APCI MS/MS） method has been established for the simultaneous determination of 24 hormones,including： testosterone,methylte-stosterone,nandrolone,nandrolone phenylpropionate,trenbolone,stanozolol,boldenone,4-androstene-3,17-dione,methandienone,norethindrone,megestrol-17-acetate,medroxyprogesterone-17-acetate,chlormadinone,17-acetate,17-alpha-hydroxyprogesterone,21-hydroxyprogesterone,medroxyprogesterone,levonorgestrel,estrone,17-beta-estradiol,estriol,17a-ethinylestradiol,hexestrol,diethylstibestrol,dienestrol.The hormones were extracted twice by ethyl acetate and cleaned up on a silica solid phase extraction column.The separation was carried out by a CAPCELL PAK C18（100mm×2.0mm i.d.,5μm） column,using methanol and water as mobile phases.Using APCI ion source,the target compounds were confirmed and quantified by MS/MS under multiple reaction monitoring（MRM） mode with an external standard.The androgens and progestogens were determined on ESI＋ mode,while the estrogens on ESI-mode.Under the optimal conditions,the limits of quantification（LOQ） were 0.5-2μg/kg,and the average recoveries were from 80% to 102%.The relative standard derivations（RSDs） ranged from 6% to 10%.This method was effective,simple and sensitive and was suitable for the simultaneous determination and confirmation of three sorts of hormones.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第5期62-67,共6页
Chinese Journal of Analysis Laboratory
基金
农业部行业标准制订、修订项目(12300)资助
