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超高效液相色谱-串联四极杆飞行时间质谱和超高效液相色谱-串联三重四极杆质谱用于血浆中苦杏仁苷及其代谢产物野黑樱苷的定性和定量分析
  • ISSN号:1000-8713
  • 期刊名称:《色谱》
  • 时间:0
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]江西中医药大学,江西南昌330004, [2]中药固体制剂制造技术国家工程研究中心,江西南昌330006, [3]中国中医科学院中药研究所,北京100700
  • 相关基金:国家重点基础研究发展计划(“973”计划)项目(2010CB530602).
中文摘要:

建立了大鼠灌胃麻杏石甘汤后血浆中苦杏仁苷、野黑樱苷的定性及定量方法。样品经液液萃取净化处理,定性采用超高效液相色谱-串联四极杆飞行时间质谱仪(UPLC-QTOF-MS / MS),经 Shim-pack XR-ODS Ⅲ色谱柱(75 mm×2.0 mm,1.6μm)分离,定量采用超高效液相色谱-串联三重四极杆质谱仪( UPLC-Q-TRAP-MS),经 Agilent C18色谱柱(50 mm×2.1 mm,1.7μm)分离,电喷雾负离子化( ESI)及 MRM 模式测定,流动相均为乙腈-0.1%( v /v)甲酸水溶液。结果显示苦杏仁苷、野黑樱苷在相应浓度范围内线性关系良好(相关系数分别为0.9990、0.9970),精密度(RSD)小于9.20%,回收率为82.33%~95.25%,检出限( LOD)约为0.50 ng / mL。本方法快速简便,为血浆样品中苦杏仁苷、野黑樱苷的定性和定量分析提供良好参考。

英文摘要:

A method was developed for the determination of amygdalin and its metabolite pru-nasin in rat plasma after intragastric administration of Maxing shigan decoction. The analytes were identified by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and quantitatively determined by ultra-high performance liquid chroma-tography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the qualitative analysis of amygdalin and prunasin in the plasma sample was performed on a Shim-pack XR-ODS Ⅲ HPLC column( 75 mm × 2. 0 mm,1. 6 μm ),using acetonitrile-0. 1%( v / v)formic acid aqueous solution. The detection was performed on a Triple TOF 5600 quadru-pole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C 18 HPLC column(50 mm ×2. 1 mm,1. 7 μm),using acetonitrile-0. 1%(v / v)formic acid aqueous solution. The detection was performed on an AB Q-TRAP 4500 triple quadrupole mass spectrometer utilizing electrospray ionization( ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM)mode. The qualitative analysis results showed that amygdalin and its metabolite pruna-sin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1. 05 - 4 200 ng / mL with the correlation coefficient of 0. 999 0 and the linear range of prunasin was 1. 25-2 490 ng / mL with the correlation coefficient of 0. 997 0. The method had a good precision with the relative standard deviations( RSDs)lower than 9. 20%and the overall recoveries varied from 82. 33% to 95. 25% . The limits of detection( LODs)of amygdalin and prunasin were 0. 50 ng / mL. With good reproducibility,the method is simple,fast and effective for the qualitative and quantitative analysis of the amygdalin and prunasin in plas-ma sample of rats which were administered by Maxing shigan d

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期刊信息
  • 《色谱》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国化学会 中国科学院大连化学物理研究所
  • 主编:张玉奎
  • 地址:大连市中山路457号
  • 邮编:116023
  • 邮箱:sepu@dicp.ac.cn
  • 电话:0411-84379021
  • 国际标准刊号:ISSN:1000-8713
  • 国内统一刊号:ISSN:21-1185/O6
  • 邮发代号:8-43
  • 获奖情况:
  • 1998年获中国科学院科学出版基金择优支持(1998-2...,2001年获第四届中国科学院优秀期刊二等奖,2002年获第三届中国科协优秀期刊三等奖,连续多年被评为辽宁省一级期刊
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),波兰哥白尼索引,荷兰文摘与引文数据库,美国生物医学检索系统,美国剑桥科学文摘,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),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:26730