Chemical Profiles and Simultaneous Quantification of Aurantii fructus by Use of HPLC-Q-TOF-MS Combined with GC-MS and HPLC Methods.

Yingjie He,Changqiao Wu,Jianguo Zeng,Suren Sooranna,Hongqi Xie,Qi Tang,Wei Wang,Yiting Shi,Zongkai Li,Yun Chen

doi:10.3390/molecules23092189

Abstract

Aurantii fructus (AF) is a traditional Chinese medicine that has been used to improve gastrointestinal motility disorders for over a thousand years, but there is no exhaustive identification of the basic chemical components and comprehensive quality control of this herb. In this study, high-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS) and gas chromatography coupled mass spectrometry (GC-MS) were employed to identify the basic chemical compounds, and high-performance liquid chromatography (HPLC) was developed to determine the major biochemical markers from AF extract. There were 104 compounds belonging to eight structure types, including 13 amino acids or peptides, seven alkaloids, 18 flavanones, 14 flavones, 15 polymethoxyflavonoids, six triterpenoids, nine coumarins, and 18 volatile oils, as well as four other compounds that were systematically identified as the basic components from AF, and among them, 41 compounds were reported for the first time. Twelve bioactive ingredients were chosen as the benchmark markers to evaluate the quality of AF. The analysis was completed with a gradient elution at a flow rate of 0.7 mL/min within 55 min. This efficient method was validated showing good linearity, precision, stability, repeatability and recovery. Furthermore, the method was successfully applied to the simultaneous determination of 12 chemical markers in different samples of AF. This study could be applied to the identification of multiple bioactive substances and improve the quality control of AF.

Highlights

Aurantii fructus (AF) is the dried and immature fruit of Citrus aurantium L. and its cultivars
The aim of this study is to establish a new comprehensive analysis method for gaining insight into the exhaustive chemical profiles of AF using high-performance liquid chromatography (HPLC)-Q-TOF-MS combined with gas chromatography coupled mass spectrometry (GC-MS)
As many as 86 compounds were identified as the main constituents from AF by electrospray ionization (ESI)-Q-TOF-MS

Summary

Introduction

Aurantii fructus (AF) is the dried and immature fruit of Citrus aurantium L. and its cultivars It plays important roles in traditional Chinese medicine (TCM) and is a functional food that has been intensively applied to treat stagnation of dyspepsia, improve gastrointestinal motility dysfunction, and alleviate chest pain in traditional therapies [1,2]. Modern pharmacological studies have shown these compounds to exhibit various activities, e.g., anti-inflammatory [9,10], anti-oxidation [10,11], regulation of gastrointestinal and prevention of cardiovascular disease [12,13], and they are considered to be the major bioactive constituents in AF. Plenty of clinical investigations have shown that the main pharmacological ingredients of AF are flavonoids, such as flavanones and polymethoxyflavonoids (PMFs), that mainly focus on regulating gastrointestinal dysmotility [12,14,15]

Objectives

Methods

Results

Conclusion