液相色谱-质谱联用法同时测定大鼠血浆中柔红霉素和汉防己甲素的浓度

发布时间：2018-04-06 07:26

本文选题：柔红霉素(DNR)　切入点：汉防己甲素(Tet)　出处：《中国医院药学杂志》2015年10期

【摘要】：目的:建立一种灵敏快速的LC-MS/MS方法,能够同时测定大鼠血浆中的柔红霉素(DNR)和汉防己甲素(Tet)含量。方法:色谱柱使用的是BDS HYPERSIL-C8柱(2.1 mm×100 mm,3μm);采用乙腈-5 mmo L·L-1醋酸铵(46∶54 V/V)作为流动相,其中含千分之四的甲酸;流速设为0.2 ml·min-1。采用醋酸乙酯对血浆样品进行液液萃取,选择阿霉素(DOX)为内标,进行HPLC-MS/MS分析,正离子扫描,MRM模式检测。DNR、Tet和IS的定量检测离子对分别为m/z 528.4→321.3,m/z 623.1→381.8,m/z 544.4→397.6。结果:大鼠血浆中检测DNR及Tet的线性范围分别为2~500 ng·ml-1,0.5~400 ng·ml-1,DNR与Tet高、中、低浓度提取回收率均86%,日内精密度RSD7.3%,日间精密度RSD4.9%,准确度RE在-0.4%~4.5%范围内。结论:本方法可灵敏、快速地测定大鼠血浆中DNR及Tet浓度。
[Abstract]:Aim: to establish a sensitive and rapid LC-MS/MS method for simultaneous determination of daunorubicin and Tetrandrine in plasma of rats.Methods: the BDS HYPERSIL-C8 column was used, the mobile phase was acetonitrile-5 mmo L L-1 ammonium acetate 46: 54 V / V, containing 4/1000 formic acid, and the flow rate was 0. 2 ml min-1.Plasma samples were extracted by ethyl acetate and doxorubicin (DOX) was selected as internal standard. HPLC-MS/MS analysis was carried out. The quantitative ion pairs were m / z 528.4 ~ 321.3m / z 623.1 ~ 381.8 m / z 544.4 397.6for positive ion scanning MRM-mode detection of .DNRTet and is, respectively.Results: the linear range for the detection of DNR and Tet in plasma of rats was 2 500 ng / ml ~ (-1) and 0.5 ~ 400 ng / ml ~ (-1) Tet, respectively. The recoveries of middle and low concentrations were 86%, the intra day precision was 7. 3%, the daytime precision was 4. 9%, and the accuracy of RE was in the range of -0. 4% and 4. 5%.Conclusion: this method is sensitive and rapid for the determination of DNR and Tet in rat plasma.
【作者单位】：南京工业大学药学院;东南大学医学院;
【基金】：江苏政府留学奖学金(2013) 国家自然科学基金资助项目(编号:81170492,81373478)
【分类号】：R927.2;O657.63

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