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紫芝超细粉超临界流体萃取物组分HPLC-ESI-MS分析

HPLC-DAD-MS analysis of the supercritical fluid extraction from ultrafine-powder of Ganoderma sinense

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【作者】 陈体强吴锦忠余德亿吴岩斌

【Author】 CHEN Ti-qiang~1 WU Jinzhong~2 YU De-yi~1 WU Yan-bin~2 (1 Fijian Academy of Agricultural Sciences,Fuzhou 350013;2 Department of TCM Pharmacology,FCTCM,Fuzhou 3500133)

【机构】 福建省农业科学院福建中医学院药学系第二军医大学药学院

【摘要】 本研究采用超临界流体萃取与高效液相色谱-离子阱质谱联用(SFE-HPLC-MS))分析(离线联用模式)紫芝子实体化学成分。在超临界CO2流体中加入10%流量的乙醇,采用超临界改性CO2流体萃取法,将紫芝子实体超细粉中(脂肪酸与挥发油、三萜类及甾体等)三类化学成分萃取出来,平均得率约为3.75%(w/w)。采用二极管阵列检测器(DAD)优化选择280nm和210nm作为检测波长(参比波长360nm),液相色谱的保留值与分离度均较好,其中以280nm得到的色谱分离最佳,主峰得到了明显的基线分离。通过HPLC-DAD分析,分别给出了萃取物全样及析出物、上清液中相对含量较丰的主要组分的色谱特征。通过电喷雾离子阱质谱(ESI-MS),采用正负离子模式质谱扫描均可得到约20个清晰的峰信号;分析确定了萃取物主要组分的分子量信息(m/z:188~614)。

【Abstract】 A off-line mode coupled supercritical fluid extraction(SFE) with high-performance liquid chromatography and electrospray ion trap mass spectrometry(HPLC-DAD-MS) analytical method was developed in this paper.Compounds of fatty acids and essential oils,steroids,triterpenoids were simultaneity extracted from the ultrafine-powder of Ganoderma sinense("Minzi 96"strain,HAMS 77207,cultivated with laburnum or branches of broadleaf tree) fruitbodies,by supercritical CO2 fluid extraction with 10%flux of ethanol as entrainer,and the average extract ratio was 3.75%(w/w). Diode-array detector(DAD)was used to choose the preferable detective wave length,and the retention and resolution of high performance liquid chromatography at 210nm/280nm(Ref.=360nm) were better,especially at 280nm,main peaks were baseline separated distinctly with good resolution for most peaks.Chromatography characteristic of main constitutes with relative abundance(percentage of peak area) were acquired and described respectively,from the supercritical fluid extraction(Total extraction,Precipitate and supernatant) by HPLC-DAD.About 20 peak signal were acquired,in positive and negative ion detection mode were analyzed by electrospray ion trap mass spectrometry(ESI-ITMS),and the molecular weight distribution(m/z:188~614) of main compounds were identified according to the molecular ions in MS spectra.

  • 【会议录名称】 中华中医药学会第九届中药鉴定学术会议论文集——祝贺中华中医药学会中药鉴定分会成立二十周年
  • 【会议名称】中华中医药学会第九届中药鉴定学术会议
  • 【会议时间】2008-07-01
  • 【会议地点】中国浙江建德
  • 【分类号】R284.1
  • 【主办单位】中华中医药学会中药鉴定分会
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