High performance liquid chromatography coupled to electrospray ionization and quadrupole time-of-flight-mass spectrometry as a powerful analytical strategy for systematic analysis and improved characterization of the major bioactive constituents from Radix Dipsaci

High performance liquid chromatography coupled to electrospray ionization and quadrupole time-of-flight-mass spectrometry as a powerful analytical strategy for systematic analysis and improved characterization of the major bioactive constituents from Radix Dipsaci
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DOI:
10.1016/j.jpba.2014.05.006
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发表时间:
2014-09-01
影响因子:
3.4
通讯作者:
Lu, Yunhua
Lu, Yunhua
中科院分区:
医学3区
文献类型:
--
作者:
Ling, Yun;Liu, Keyue;Lu, Yunhua

文献摘要

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续断(Rd)是续断属植物的干燥根,是治疗骨病的常用中药,具有强骨、骨愈合的作用。然而,该植物中多种化合物的高极性、非生色团和低丰度给它们的分离和结构鉴定带来了困难,这阻碍了RD在临床上的应用,并延缓了RD现代化的进程。本工作采用灵敏、快速的高效液相色谱-电喷雾飞行时间-质谱联用(HPLC-ESI-QTOF-MS/MS)联用技术,对白术中多种次要成分进行快速分离鉴定。采用Agilent Poroshell120 EC-C18色谱柱(2.1 mm×100 mm,i.d.,2.7微米),以0.1%甲酸水溶液和乙腈为流动相,梯度洗脱。结果共鉴定或初步鉴定了川续断皂苷、环烯醚萜苷和咖啡酰奎宁酸衍生物等36个主要成分,其中11个未见文献报道。综上所述,高效液相色谱-电喷雾飞行时间-质联用联用技术是分离鉴定中药复杂基质中有效成分的一种可行、可靠的方法。(C)2014爱思唯尔B.V.保留所有权利。
Radix Dipsaci (RD), the dried root of Dipsacus asper, is commonly used as a traditional Chinese medicine for the treatment of bone diseases and functions in strengthening bone and healing bone fractures. Nevertheless, the high polarity, non chromophores and low abundance of multiple compounds in this plant bring difficulty for their isolation and structural determination by traditional chromatographic and spectroscopic techniques, which hindered the use of RD in clinical practice and retarded the process of RD modernization. In this work, a sensitive and rapid high-performance liquid chromatography coupled with electrospray time-of-flight-mass spectrometry (HPLC-ESI-QTOF-MS/MS) was employed to rapidly separate and identify the multiple minor constituents in RD. Separation was performed an Agilent poroshell 120 EC-C18 column (2.1 mm x 100 mm, i.d., 2.7 mu m) with 0.1% formic acid aqueous solution and acetonitrile as the mobile phase under gradient conditions. As a result, 36 major constituents including dipsacus saponins, iridoid glycosides and caffeoyl quinic acid derivatives were identified or tentatively characterized from the RD, 11 of which had not been previously reported to the best of our knowledge. In conclusion, the HPLC-ESI-QTOF-MS/MS is feasible and credible technique to separate and identify the constituents in complex matrices of traditional Chinese medicines. (C) 2014 Elsevier B.V. All rights reserved.