色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1032-1039.DOI: 10.3724/SP.J.1123.2015.06013

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定银杏保健茶中的16种黄酮类功效成分

蒋娅兰1,2, 黄芳3, 毋福海2, 吴惠勤3, 黄晓兰3, 邓欣3   

  1. 1. 广东药学院中药学院, 广东 广州 510006;
    2. 广东药学院公共卫生学院, 广东 广州 510024;
    3. 中国广州分析测试中心, 广东省分析测试技术公共实验室, 广东 广州 510070
  • 收稿日期:2015-06-08 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 毋福海
  • 基金资助:

    广东省科技成果转化启动项目(2011A060903001).

Simultaneous determination of 16 flavonoids in the ginkgo dietary supplement tea by high performance liquid chromatography-tandem mass spectrometry

JIANG Yalan1,2, HUANG Fang3, WU Fuhai2, WU Huiqin3, HUANG Xiaolan3, DENG Xin3   

  1. 1. College of Traditional Chinese Medicine, Guangdong Pharmaceutical University, Guangzhou 510006, China;
    2. School of Public Health, Guangdong Pharmaceutical University, Guangzhou 510024, China;
    3. Guangdong Provincial Public Laboratory of Analysis and Testing Technology, China National Analytical Center (Guangzhou), Guangzhou 510070, China
  • Received:2015-06-08 Online:2015-10-08 Published:2012-05-09

PDF

194

摘要：

建立了银杏保健茶中16种黄酮类物质的液相色谱-串联质谱(LC-MS/MS)测定方法。16种黄酮成分分别为儿茶素、牡荆素、葛根素、大豆苷元、水飞蓟宾、槲皮素、木犀草素、芹菜素、柚皮素、橙皮素二氢查尔酮、山柰酚、橙皮素、异鼠李素、黄芩素、川陈皮素、桔皮素。实验优化了液相色谱条件和质谱参数。采用C18柱分离,流动相为乙腈-水(含0.1%甲酸)梯度洗脱,流速0.25 mL/min,以电喷雾离子源正离子多反应监测(MRM)模式进行MS/MS检测。16种黄酮类物质在各自的线性范围内具有良好的线性关系,相关系数大于0.996,低、中、高3个添加水平的平均回收率在70.9%~100.0%之间,相对标准偏差小于10%。通过检测发现实际样品中9种黄酮物质含量较高,分别是:山柰酚、槲皮素、橙皮素、牡荆素、木犀草素、儿茶素、芹菜素、柚皮素、异鼠李素,占总量的99.6%,此9种物质可作为银杏保健茶的质量控制指标。本法简便、快速、准确可靠,可用于控制银杏保健茶的质量。

关键词: 黄酮, 液相色谱-串联质谱, 银杏保健茶

Abstract:

A method for the determination of 16 functional components of ginkgo dietary supplement tea such as catechin, vitexin, puerarin, isoflavoues aglycone, silymarin, quercetin, luteolin, apigenin, naringenin, hesperitin dihydrochalcone, kaempferol, hesperitin, isorhamnetin, baicalein, nobiletin and tangeretin by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was proposed. The conditions of chromatography and mass spectrometry were optimized. The 16 flavonoids were separated on a C18 chromatographic column with acetonitrile and water (additional 0.1% formic acid) as mobile phases under gradient elution at a flow rate of 0.25 mL/min. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. Good linearities for all the compounds, with correlation coefficients over 0.996, were acquired. The recoveries were in the range of 70.9% to 100.0% (n=6), while the relative standard deviations (RSDs) were less than 10%. The results showed that the nine flavonoids, which were kaempferol, quercetin, hesperitin, vitexin, luteolin, catechin, apigenin, naringenin and isorhamnetin, were higher in contents among the 16 flavonoids in real samples, and they constituted up to 99.6% of the total flavonoids. The contents of these nine flavonoids can be considered as the quality control index of the ginkgo dietary supplement tea. The method proved to be rapid, selective, sensitive and stable, and it can be applied to control the quality of the ginkgo dietary supplement tea.

Key words: flavonoids, ginkgo dietary supplement tea, liquid chromatography-tandem mass spectrometry (LC-MS/MS)

中图分类号: