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作 者:赵燕燕[1,2] 高茜[2] 李月秋[1] 韩媛媛[1] 刘丽艳[1]
机构地区:[1]河北大学医学实验中心,河北保定071000 [2]河北大学化学与环境科学学院,河北保定071002
出 处:《河北大学学报(自然科学版)》2012年第1期47-51,共5页Journal of Hebei University(Natural Science Edition)
基 金:河北省科技攻关项目(05276101D-88);河北省教育厅科学研究计划项目(2009315);河北省卫生厅医学科学研究重点课题计划项目(20090570);河北省中医药管理局科研计划课题(2008072)
摘 要:采用反相高效液相色谱法检测人体血浆中替勃龙的含量.以5倍样品体积的乙腈萃取2次,经氮气吹干,甲醇溶解后,上机分析.采用Promosil-C18色谱柱(4.6mm×250mm,5μm),流动相:甲醇-乙腈-水,流速:1.0mL/min,进样量:10μL,检测波长:204nm,柱温:25℃.在优化的色谱条件下,替勃龙在0.5~250.0μg/mL内线性关系良好(r=0.999 9),最低检测限为0.05μg/mL,平均回收率(n=3)为92.7%,RSDs小于1.6%.本方法简单,灵敏,准确,适合于体内替勃龙含量的检测与分析.A method of reversed-phase high performance liquid chromatography(RF-HPLC) was developed for the determination of tibolone in the plasma of people.The samples were extracted twice with 5 times voloum of acetonitrile.After the solvent was removed with nitrogen,the residues were dissolved in methanol.The separation column was Promosil-C18(250 mm×4.6 mm,5 μm) and the mobile phase was V(methanol)∶V(acetonitrile)∶V(water)(50∶30∶20),The flow rate was 1.0 mL/min,The injection volume was 10 μL and the detection wavelength was set at 204 nm,The column temperature was 25 ℃.Under the optimized separation conditions,the calibration curves showed good linearity within the concentrations of 0.5-250.0 μg/mL(r=0.999 9),The limit of detection was 0.05 μg/mL,The average recovery(n=3) was 92.7%,and the RSDs were less than 1.6%.This method is simple,sensitive and accurate,and suitable for the determination of tibolone in biological samples.
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