色谱

色谱 ›› 2019, Vol. 37 ›› Issue (2): 201-206.DOI: 10.3724/SP.J.1123.2018.10008

• 研究论文 • 上一篇    下一篇

高分辨采样二维液相色谱法同时测定金银花中绿原酸和木犀草苷含量

王智聪, 傅荣杰, 吉建国, 陈波   

  1. 安捷伦科技(上海)有限公司, 上海 200131
  • 收稿日期:2018-10-09 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 王智聪,E-mail:zhi-cong.wang@agilent.com

Simultaneous determination of chlorogenic acid and cynaroside contents in Lonicerae Japonica Flos by high resolution sampling two-dimensional liquid chromatography

WANG Zhicong, FU Rongjie, JI Jianguo, CHEN Bo   

  1. Agilent Technology(Shanghai) Co., Ltd, Shanghai 200131, China
  • Received:2018-10-09 Online:2019-02-09 Published:2014-12-31

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摘要：

采用高分辨采样二维液相色谱法（HiRes 2D-LC）对金银花中绿原酸和木犀草苷进行准确定量分析。第一维液相色谱采用C18色谱柱，以乙腈和0.4%（v/v）磷酸水溶液为流动相进行梯度洗脱；第二维液相色谱采用SB-Phenyl色谱柱，以乙腈和0.5%（v/v）乙酸水溶液为流动相进行梯度洗脱；二维接口采用五位十通阀，并配置2个多中心切割阀，对绿原酸组分和木犀草苷组分进行多次连续切割。实验结果表明，二维液相色谱分析提高了绿原酸和木犀草苷色谱峰的确认能力，可揭示一维液相色谱分析中共洗脱或隐藏峰的信息；高分辨采样模式实现了一维目标组分的片段式整峰切割，提高了二维液相色谱分析的准确定量能力；通过线性关系、基质加标回收和重复性等考察结果，表明高分辨采样二维液相色谱具有优异的定量准确性和重复性，为中药等复杂基质组分样品的分离和准确定量提供了新方法。

关键词: 定量分析, 峰纯度确认, 高分辨采样二维液相色谱, 金银花, 绿原酸, 木犀草苷, 中药

Abstract:

An innovative analytical method based on high resolution sampling two-dimensional liquid chromatography (HiRes 2D-LC) was established for determination of chlorogenic acid and cynaroside in Lonicerae Japonica Flos. A C18 column was used in the first dimension (1D)-LC separation with acetonitrile and 0.4% (v/v) phosphoric acid aqueous solution as mobile phases. Five heart cuts of chlorogenic acid and four heart cuts of cynaroside were stored in 2D-LC interface, which was a 5-position-10-port valve equipped with two multiple heart-cutting valves. The stored cuts were sequentially separated in the second dimension (2D)-LC. The 2D separation was carried out on an SB-Phenyl column with acetonitrile and 0.5% (v/v) acetic acid aqueous solution as mobile phases. The results showed that chlorogenic acid peaks in the 1D were well separated, whereas cynaroside peaks in the 1D were co-eluted with interferences. The above two targets were accurately quantified through a high resolution sampling mode based on continuous slice cuts of the whole target peaks. The method had good linearity, recovery and repeatability. The HiRes 2D-LC system could be used to improve separation and quantification of (un)targets in traditional Chinese medicine samples.

Key words: Lonicerae Japonica Flos, chlorogenic acid, cynaroside, high resolution sampling two-dimensional liquid chromatography (HiRes 2D-LC), peak purity confirmation, quantitative analysis, traditional Chinese medicine (TCM)

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