食品科学

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超高效液相-串联四极杆质谱联用法同时测定并比较甘草各部位中8 种成分含量

叶日贵1,高 杰1,王 冰1,李二虎1,张 燕1,江 飞1,曹 瑞1,服部征雄2,王世明3,马超美1,*   

  1. 1.内蒙古大学生命科学学院,内蒙古 呼和浩特 010021;2.日本富山大学和汉医药学综合研究所,
    日本 富山 2630 930-0194;3.内蒙古鄂尔多斯蓝原中药材有限公司,内蒙古 鄂尔多斯 150600
  • 出版日期:2014-10-25 发布日期:2014-11-07
  • 基金资助:

    内蒙古大学本科生创新基金项目

Simultaneous Quantification and Comparison of 8 Components in Different Parts of Glycyrrhiza uralensis Using Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

YE Ri-gui 1, GAO Jie 1, WANG Bing 1, LI Er-hu1, ZHANG Yan1, JIANG Fei1, CAO Rui1, HATTORI Masao2, WANG Shi-ming3, MA Chao-mei1,*   

  1. 1. School of Life Sciences, Inner Mongolia University, Huhhot 010021, China; 2. Institute of Natural Medicine,
    University of Toyama, Toyama 2630 930-0194, Japan; 3. Erdos Lan Yuan Materia Medica Co. Ltd., Erdos 150600, China
  • Online:2014-10-25 Published:2014-11-07

摘要:

建立同时检测甘草中8 种成分:22-羟基-甘草次酸、3-epi-甘草次酸、甘草次酸、甘草酸、甘草苷、芒柄花黄素、异甘草酚、甘草香豆素的超高效液相色谱-串联四极杆质谱联用法。选用胆酸作为三萜成分的内标,相思子素2”-O-β-芹菜糖苷作为酚类化合物的内标。甘草样品经粉碎用甲醇(含内标液)超声提取,采用安捷伦ZORBAXRRHD C18柱(50 mm×2.1 mm,1.8 μm),以甲醇-0.1%甲酸溶液为流动相,梯度洗脱,以电喷雾电离源,采用超高效液相-串联四极杆质谱联用动态多反应监测模式测定。结果表明,8 种成分检出限均小于0.048 8 μg/mL,定量限均小于0.195 2 μg/mL,在0.048 8~12.500 0、0.048 8~12.500 0、0.012 2~12.500 0、0.048 8~50.000 0、0.048 8~50.000 0、0.012 2~12.500 0、0.012 2~15.000 0、0.195 2~12.500 0 μg/mL范围内,22-羟基-甘草次酸、3-epi-甘草次酸、甘草次酸、甘草酸、甘草苷、芒柄花黄素、异甘草酚、甘草香豆素的峰面积与质量浓度呈良好线性关系,相关系数均大于0.99;方法回收率为97.2%~113.0%间;其日内及日间精密度实验的相对标准偏差分别为 2.63%~4.47%及1.75%~3.72%。该方法灵敏度高、稳定性强、操作简便、快捷、准确,可用于甘草各部位及其相关食品质量控制。

关键词: 甘草, 甘草各部位, 超高效液相色谱-串联四极杆质谱联用, 同时测定

Abstract:

An ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS)
with dynamic multiple reaction mode was developed to simultaneously quantify 8 constituents including 22-hydroxyglycyrrhetinic
acid, 3-epi-glycyrrhetinic acid, glycyrrhetinic acid, glycyrrhizic acid, liquiritin, glycycoumarin, formononetin
and isoglycyrol in Glycyrrhiza uralensis. Cholic acid and abrusin 2”-O-β-apioside were used as the internal standards for
triterpenoid and phenolic components, respectively. The internal standards were added to methanol before being used to
extract samples. The separation was performed on an Agilent ZORBAX RRHD Eclipse Plus C18 column (50 mm × 2.1 mm,
1.8 μm) with methanol-0.1% formic acid as the mobile phase at a flow rate of 0.4 mL/min. As a result, the linear ranges of
22-hydroxy-glycyrrhetinic acid, 3-epi-glycyrrhetinic acid, glycyrrhetinic acid, glycyrrhizic acid, liquiritin, formononetin,
isoglycyrol and glycycoumarin were 0.048 8–12.500 0, 0.048 8–12.500 0, 0.012 2–12.500 0, 0.048 8–50.000 0, 0.048 8–
50.000 0, 0.012 2–12.500 0, 0.012 2–15.000 0 and 0.195 2–12.500 0 μg/mL, respectively, with correlation coefficients higher than
0.99. The average recovery rate of the developed method ranged from 97.2% to113.0% and the intra-day and inter-day relative
standard deviations (RSDs) were 2.63%–4.47% and 1.75%–3.72%, respectively. This method is sensitive, simple, fast, and
accurate, and can be used for the quality control of different parts of Glycyrrhiza uralensis and related food products.

Key words: Glycyrrhiza uralensis, different parts of Glycyrrhiza uralensis, ultra-high-performance liquid chromatographytriple quadrupole mass spectrometry (UPLC-QQQMS), simultaneous determination

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