色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 591-599.DOI: 10.3724/SP.J.1123.2014.01021

• 研究论文 • 上一篇    下一篇

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

高萌1, 王跃生3, 魏惠珍1, 欧阳辉2, 何明珍2, 曾恋情1, 申峰云1, 郭强1, 饶毅1   

  1. 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
  • 收稿日期:2014-01-13 修回日期:2014-03-14 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 饶毅
  • 基金资助:

    国家重点基础研究发展计划（“973”计划）项目（2010CB530602）.

Qualitative and quantitative analysis of amygdalin and its metabolite prunasin in plasma by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry

GAO Meng1, WANG Yuesheng3, WEI Huizhen1, OUYANG Hui2, HE Mingzhen2, ZENG Lianqing1, SHEN Fengyun1, GUO Qiang1, RAO Yi1   

  1. 1. Jiangxi University of Chinese Traditional Medicine, Nanchang 330004, China;
    2. The National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine, Nanchang 330006, China;
    3. Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China
  • Received:2014-01-13 Revised:2014-03-14 Online:2014-06-08 Published:2014-05-22

PDF

532

被引次数

6

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，1.6 μm）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，1.7 μm）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。

关键词: 超高效液相色谱-串联三重四极杆质谱, 超高效液相色谱-串联四极杆飞行时间质谱, 大鼠血浆, 苦杏仁苷, 野黑樱苷

Abstract:

A method was developed for the determination of amygdalin and its metabolite prunasin 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 chromatography-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 quadrupole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C18 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 prunasin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1.05-4200 ng/mL with the correlation coefficient of 0.9990 and the linear range of prunasin was 1.25-2490 ng/mL with the correlation coefficient of 0.9970. 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 plasma sample of rats which were administered by Maxing shigan decoction.

Key words: amygdalin, prunasin, rat plasma, ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (UPLC-QTOF-MS/MS), ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-Q-TRAP-MS)

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