在线提取-高效液相色谱-二极管阵列检测-四极杆飞行时间质谱法快速鉴定陈皮中黄酮类化合物

doi:10.3724/SP.J.1123.2017.11031

色谱 ›› 2018, Vol. 36 ›› Issue (3): 278-284.DOI: 10.3724/SP.J.1123.2017.11031

在线提取-高效液相色谱-二极管阵列检测-四极杆飞行时间质谱法快速鉴定陈皮中黄酮类化合物

童超英¹, 彭密军², 施树云¹

1. 中南大学化学化工学院, 湖南长沙 410003;
2. 广东省测试分析研究所, 中国广州分析测试中心, 广东广州 510070

收稿日期:2017-11-20 出版日期:2018-03-08 发布日期:2018-04-04
通讯作者: 施树云,E-mail:shishuyun@126.com
基金资助:
国家自然科学基金（31660181）；广东省科学院创新驱动专项项目（2017GDASCX-0702）.

Rapid identification of flavonoid compounds in Pericarpium Citri Reticulatae by online extraction-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry

TONG Chaoying¹, PENG Mijun², SHI Shuyun¹

1. College of Chemistry and Chemical Engineering, Central South University, Changsha 410003, China;
2. Guangdong Institute of Analysis, China National Analytical Center(Guangzhou), Guangzhou 510070, China

Received:2017-11-20 Online:2018-03-08 Published:2018-04-04
Supported by:
National Natural Science Foundation of China (No. 31660181); Guangdong Academy of Sciences (GDAS) Special Project of Science and Technology Development (No. 2017GDASCX-0702).

摘要/Abstract

摘要：

建立了简便、高效的在线提取-高效液相色谱-二极管阵列-四极杆飞行时间质谱法（OLE-HPLC-DAD-QTOF-MS）快速提取和分离鉴定陈皮中黄酮类化合物。在线提取体系中，将填有陈皮粉末样品（2.0 mg）的固相萃取小柱取代样品环连接在手动进样阀上，样品直接被流动相提取并进入HPLC-DAD-QTOF-MS系统分析，无需额外的样品前处理步骤。与传统的溶剂回流提取法相比，在线提取法具有较高的提取率。通过分析化合物的紫外谱图、色谱保留时间和质谱信息，共鉴定出24种黄酮类化合物，其中新圣草次苷、柠檬黄素-3-O-（3-羟基-3-甲基戊二酸）-葡萄糖苷及其异构体首次在陈皮中报道。建立的方法为中药复杂体系中活性成分的快速分离鉴定提供了新的研究思路。

关键词: 陈皮, 高效液相色谱, 黄酮类化合物, 鉴定, 四极杆飞行时间质谱, 在线提取

Abstract:

A simple method was developed for the rapid extraction, separation and identification by online extraction (OLE) coupled with high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry (HPLC-DAD-QTOF-MS). For OLE strategy, a guard column filled with Pericarpium Citri Reticulatae powder (2.0 mg) was connected to manual injection valve by replacing the sample loop. Components were directly extracted and transferred to HPLC-DAD-QTOF-MS system by mobile phases without any extra operation. In comparison with offline heat-reflux extraction, OLE strategy presented higher extraction efficiency. A total of twenty-four flavonoid compounds were detected from Pericarpium Citri Reticulatae according to their retention times, UV spectra, accurate molecular masses, and fragment ions in MS/MS spectra. Neoeriocitrin, limocitrin-3-O-(3-hydroxy-3-methylglutarate)-glucoside and its isomer were discovered for the first time. It is concluded that the developed method offers new perspectives for the rapid separation and identification of natural products.

Key words: Pericarpium Citri Reticulatae, flavonoid compounds, high performance liquid chromatography (HPLC), identification, online extraction (OLE), quadrupole time-of-flight mass spectrometry (QTOF-MS)

中图分类号:

O658

童超英, 彭密军, 施树云. 在线提取-高效液相色谱-二极管阵列检测-四极杆飞行时间质谱法快速鉴定陈皮中黄酮类化合物[J]. 色谱, 2018, 36(3): 278-284.

TONG Chaoying, PENG Mijun, SHI Shuyun. Rapid identification of flavonoid compounds in Pericarpium Citri Reticulatae by online extraction-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(3): 278-284.

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在线提取-高效液相色谱-二极管阵列检测-四极杆飞行时间质谱法快速鉴定陈皮中黄酮类化合物

Rapid identification of flavonoid compounds in Pericarpium Citri Reticulatae by online extraction-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry

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