中国药业2017，Vol.26Issue(8)：17-20,4.DOI:10.3969/j.issn.1006-4931.2017.08.005
超高效液相色谱-串联质谱法同时测定动物类药材中4种雌激素残留
Determination of 4 Estrogens Residue in Animal Medicinal Herbs by UPLC-MS/MS
摘要
Abstract
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method for determination of 4 estrogens(estrone,diethylstilbestrol,hexoestrol,dienoestrol) residue in animal medicinal herbs. Methods The sample was enzymolyzed by adding β-glycuronidase,extrated by methanol-sodiumacelate butler satt,purified by Carb and NH2 pillaret. The ex-tract was separated on an Agilent SB-C18 column (150 mm × 2. 1 mm,1. 8 μm)with gradient elution using a mobile phase consisting of acetonitrile-water. The column temperature was 35℃. The multiple reaction monitoring(MRM)was used for monitoring,and the iso-tope internal standard method was used for quantifying. Results The calibration curve for 4 estrogens displayed good linearity in the range of 1-200 ng/mL(r > 0. 9985). The limit of detection of the proposed method was 1. 5 μg/kg,the recoveries were 70% -110%,RSD was 4. 2% -15. 1%. Conclusion The method has high sensitivity and good reproducibility,which can be suitable for the determination of 4 estrogens residue in animal medicinal herbs.关键词
超高效液相色谱-串联质谱/雌酮/己烯雌酚/己烷雌酚/己二烯雌酚/残留测定/动物类药材Key words
UPLC-MS/MS/estrone/diethylstilbestrol/hexoestrol/dienoestrol/residue delermination/animal medicinal herbs分类
医药卫生引用本文复制引用
周文杰,张治军,马娜妹..超高效液相色谱-串联质谱法同时测定动物类药材中4种雌激素残留[J].中国药业,2017,26(8):17-20,4.基金项目
广西食品药品监督管理局科研项目[桂食药监科评[ 2015 ] 20号]. （）
