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

作　　者：周文杰[1] 张治军[1] 马娜妹 

机构地区：[1]广西壮族自治区桂林食品药品检验所,广西桂林541002 [2]桂林医学院,广西桂林541004

出　　处：《中国药业》2017年第8期17-20,共4页China Pharmaceuticals

基　　金：广西食品药品监督管理局科研项目[桂食药监科评[2015]20号]

摘　　要：目的建立同时测定动物类药材中4种雌激素(雌酮、己烯雌酚、己烷雌酚和己二烯雌酚)残留的超高效液相色谱-串联质谱(UPLC-MS/MS)法。方法样品加β-葡萄糖醛酸酶酶解后,甲醇-乙酸钠缓冲盐提取,用Carb小柱和NH_2小柱净化。色谱柱为Agilent SB-C_(18)柱(150 mm×2.1 mm,1.8μm),流动相为乙腈-水,梯度洗脱,柱温为35℃。以负离子多反应监测(MRM)模式监测,同位素内标法定量。结果 4种雌激素质量浓度在1~200 ng/m L的范围内均与峰面积线性关系良好,相关系数r均大于0.998 5,方法检测限均为1.5μg/kg,平均回收率均为70%~110%,相对标准偏差(RSD)为4.2%~15.1%。结论该法灵敏度高、重复性好,可用于动物药材中4种雌激素药物残留的测定。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 

分 类 号：R914.1[医药卫生—药物化学] R931.74[医药卫生—药学]