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

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-QTOFMS)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。

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 M^^MS spectra.Neoeriocitrin,limocitrin-3-O-(3-hydroxy-3-meth-ylglutarate)-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