Subject Area物理化学
Rapid Identification of Monoterpene Glycosides in Paeoniae Radix extract using HPLC-DAD-MS/MS
Li XL(李秀玲); Xiao HB(肖红斌); Liang XM(梁鑫淼); Xiao Hongbin
Conference NameThe fourth international symposium of natural medicine and microflora
Conference Date2002-7-27
Conference Place日本
Alternative Title利用高效液相色谱-二极管阵列紫外扫描检测器-串联质谱快速识别赤芍中单萜甙类化合物
Funding Organization日本和汉医药学会
AbstractRapid Identification of Monoterpene Glycosides in Paeoniae Radix extract using HPLC-DAD-MS/MS Li Xiuling, Xiao Hongbin, Liang Xinmiao Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116011, China Paeoniae radix, derived from the roots of paeoniae species, is an herbal drug in Chinese Prescriptions widely used as anticoagulant, antiinflammatory, analgesic and sedative agent [1]. The main bioactive components in Paeonia species are monoterpene glycosides possessing a ‘cage-like ’pinane skeleton [2]. To determine monoterpene glycosides in the Paeoniae radix extract, some techniques and methods like HPTLC, HPLC, and MEKC etc were developed [3-5]. However, these methods were in need of time-consuming pretreatment procedure and rare reference standards. And the entire monoterpene glycodises analysis is impossible with these methods (up to five compounds). We present here a High-performance Liquid Chromatography –Photodiode Array Detector-Tandem Mass Spectrometry (HPLC-DAD-MS/MS) method for rapid identification of all monoterpene glycosides in the entire Paeoniae radix extract. A 5.0g pulverized Paeoniae radix was refluxed with 95% ethanol. After the extract was concentrated and filtered it was directly injected to HPLC-DAD-MS/MS system for identification of monoterpene glycosides. The HPLC analysis was performed on a Waters 2690-996 DAD system eluted with a gradient program consisting of aqueous 12 mM NH4Ac and acetonitrile (The detailed condition was shown in Fig. 1.) APCI-MS/MS analysis was carried out with Finnigan TSQ system. And HPLC-APCI-MS analysis was performed both in the positive and negative ion modes from m/z 100 to 1000 in a single run to determine the molecular mass. With the aid of paeoniflorin reference standard, the molecular ion formation and fragment pattern under CID condition for monoterpene glycosides were studied. And negative product-ion spectra (CID energy ~25eV) were applied to identify the monoterpene glycosides in the extract. According to their molecular weight and characteristic fragments, eight of the monoterpene glycosides reported previously in the sample were identified rapidly. They were debenzoylpaeoniflorin (1), oxypaeoniflorin (2), mudanpioside E (3), paeoniflorin (4), albiflorin (5), lactiflorin (6), benzoyloxypaeonflorin (7), and benzoylpaeoniflorin (8). Two components, which were not reported in Paeoniae radix, were also been characterized. Their possible structures were postulated on the basis of their [M-H]- product ion spectra and UV spectra. One (P2) was identified tentatively as Ortho- Oxypaeoniflorin (isomer of 2) and the M.W. of the other (P1) was 446. The detailed results were shown in Fig.1 and Table 1.
Document Type会议论文
Corresponding AuthorXiao Hongbin
Recommended Citation
GB/T 7714
Li XL,Xiao HB,Liang XM,et al. Rapid Identification of Monoterpene Glycosides in Paeoniae Radix extract using HPLC-DAD-MS/MS[C],2002:40/2.
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