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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
  • ISSN号:1001-5213
  • 期刊名称:《中国医院药学杂志》
  • 时间:0
  • 分类:R927.2[医药卫生—药学]
  • 作者机构:[1]南京工业大学药学院,江苏南京211816, [2]东南大学医学院,江苏南京210009
  • 相关基金: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)
中文摘要:

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RSD〈7.3%,日间精密度RSD〈4.9%,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。

英文摘要:

OBJECTIVE To investigate pharmacokinetics of daunorubicin (DNR) and tetrandrine (Tet) alone or in combina- tion in healthy rats by using liquid chromatography with tandem mass spectrometry method developed and validated for quantifi- cation of DNR and Tet in rat plasma. METHODS A BDS HYPERSIL-C8 column (2. 3 mm× 75 mm, 3 μm) was used with a mobile phase consisted of acetonitrile, 5 rnmoL-L-t ammonium acetate and 0. 04% formic acid (46: 54, V/V) at a flow rate of 0. 2 ml.min 1. Plasma samples were pretreated by liquid-liquid extraction with ethyl acetate and doxorubicin as internal stand- ard (IS). The detection was performed using a mass spectrometer by multiple reaction monitoring (MRM) using positive ioniza- tion. The transitions monitored for DNR, Tet and IS were m/z 528→363. 1, m/z 623. 4→381.1 and m/z 544. 3→397.3, re- spectively. RESULTS Calibration curve was linear and validated over a concentration range of 2 - 500 ng. ml^-1 for DNR and 0. 5- 400 ng·ml^-1 for Tet. The inter-day precisions (RSD) were within 7. 3% and intra-day preeisions (RSD) were within 4. 9%, while the accuracy (R. E. ) values were ranged from -0. 4 % to 4. 5 % in plasma. The recoveries obtained for DNR and Tet were more than 86%. CONCLUSION LC-MS/MS method is sensitive, rapid and selective for simultaneous determination of DNR and Tet in rat plasma, and can be successfully applied to pharmacokinetic study.

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期刊信息
  • 《中国医院药学杂志》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国药学会
  • 主编:陈华庭
  • 地址:武汉市汉口胜利街155号
  • 邮编:430014
  • 邮箱:pharmacy@vip.163.com
  • 电话:027-82836596
  • 国际标准刊号:ISSN:1001-5213
  • 国内统一刊号:ISSN:42-1204/R
  • 邮发代号:38-50
  • 获奖情况:
  • 曾获中国药学会优秀期刊二等奖,中国科协优秀期刊三等奖,湖北省优秀期刊奖
  • 国内外数据库收录:
  • 美国国际药学文摘,美国化学文摘(网络版),日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),中国北大核心期刊(2000版)
  • 被引量:53772