生附片化学成分的HPLC/ESI-MS~n研究

采用高效液相色谱与电喷雾质谱联用技术,对生附片的化学成分进行了系统的研究.并辅以提取离子色谱方法.发现微量的化学成分.通过保留时间,质荷比及多级串联质谱数据,共鉴定了48个成分,其中双酯型生物碱8个,单酯型生物碱7个,脂型生物碱29个.其中双酯型生物碱是生附片中的主要成分,而单酯型和脂型生物碱的含量和种类较少.

西洋参与北沙参的HPLC、ESI-MS指纹图谱识别

目的:通过HPLC、ESI-MS指纹图谱对中药西洋参与北沙参进行鉴别。方法:利用HPLC和ESI-MS技术,优化西洋参、北沙参提取物的色谱和质谱分离分析条件,建立二者HPLC、ESI-MS指纹图谱。结果:确定出西洋参与北沙参HPLC的各色谱峰相对保留时间;根据MS图中各成份的m/z值,确定相应成分的分子量。二者的液相色谱和质谱指纹图谱完全不同。结论:通过HPLC、ESI-MS指纹图谱可以完全鉴别中药西洋参与北沙参,方法简单准确,重现性好,具有实用价值。

刺五加叶的HPLC-UV和ESI-MS指纹图谱研究

对12批不同来源的刺五加叶提取物进行指纹图谱研究,并利用ESI-MS指纹图谱鉴别刺五加叶与山楂叶。分别采用高效液相色谱(HPLC-UV)和电喷雾电离质谱(ESI-MS)测定12批不同来源的刺五加叶提取物,利用ESI-MS技术测定刺五加叶与山楂叶提取物,得到了分离度、精密度和重现性均较好的刺五加叶HPLC-UV及ESI-MS指纹图谱;同时,利用刺五加叶与山楂叶ESI-MS指纹图谱的差异,成功鉴别了二者,可为刺五加叶药材的质量控制提供参考。

麻黄炮制条件的ESI-MS法优化

ESI-MS was used to optimize the Ephedra sinica refinement. The ratio of honey to drug is 20/100, and the ratio of water to honey is 1/2. The toast temperature is 80 ℃, and the toast time is 2 h. The change of Ephedra sinica after processing was given.

Studies on Triterpenoids and Flavones in Glycyrrhiza uralensis Fisch by HPLC-ESI-MSn and FT-ICR-MSn

Seven compounds, four flavones and three triterpenoids from Glycyrrhiza uralensis Fisch. extract are identified by high performance liquid chromatography coupled with electrospray ionization multi-tandem mass spectrometry (HPLC-ESI-MSn). The fragmentation pathways of these compounds are investigated by ESI-MSn and Fourier transform ion cyclotron resonance multiple-stage tandem mass spectrometry (FT-ICR-MSn). Comparing the retention times (t(R)) and mass spectra with those of reference compounds, seven components are identified in Glycyrrhiza uralensis Fisch. and their MSn data proposed plausible schemes for their fragmentation. All the experimental results show that ESI-MSn and FT-ICR-MSn are powerful tools for the structural characterization of triterpenoids and flavones

ESI-MS和HPLC-UV法研究大黄、黄柏、赤芍炮制前后化学成分变化

目的:考察大黄、黄柏、赤芍炮制前后化学成分在质和量方面的变化,以探讨中药的炮制机理。方法:利用电喷雾质谱法(ESI-MS)和高效液相色谱法(HPLC-UV),对大黄、黄柏、赤芍炮制前后的化学成分进行详细研究。质谱:电喷雾电离源(ESI),加热毛细管温度为200℃,喷雾电压为4.5kV;液相色谱:色谱柱为Agilent Zorbax C18柱(4.6mm×150mm,5μm),柱温均为28℃。结果:大黄经酒制和醋制后,其化学成分的含量变化较大;黄柏经酒制后巴马汀的含量略有增加,而小檗碱的含量呈下降趋势;盐制对于黄柏的化学成分几乎无影响;赤芍经酒制和炒制后,芍药苷的含量都呈下降趋势。结论:不同炮制方法对化学成分的影响不同,为进一步阐明中药材炮制入药的科学内涵提供了实验依据。

Evaluation of Effects of Bivalent Cations on the Formation of Purine-rich Triple-Helix DNA by ESI-FT-MS

The GGA triplet repeats are widely dispersed throughout eukaryotic genomes. (GGA)n or (GGT)n oligonucleotides can interact with double-stranded DNA containing (GGA:CCT)n to form triple-stranded DNA. The effects of 8 divalent metal ions (3 alkaline-earth metals and 5 transition metals) on formation of these purine-rich triple-helix DNA were investigated by electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FT-MS). In the absence of metal ions, no triplex but single-strand, duplex, and purine homodimer ions were observed in mass spectra. The triple-helix DNA complexes were observed only in the presence of certain divalent ions. The effects of different divalent cations on the formation of purine-rich triplexes were compared. Transition-metal ions, especially Co2+ and Ni2+, significantly boost the formation of triple-helix DNA, whereas alkaline-earth metal ions have no positive effects on triplex formation. In addition, Ba2+ is notably beneficial to the formation of homodimer instead of triplex.

复方板蓝根颗粒水提部位的ESI-MS指纹图谱研究

Sialic acid and lysine as an internal standard substance,the ESI-MS fingerprinting of extracts of Compound Indigowoad Root Granule which from different origin was studied.The fingerprinting was obtained with better precision and reproducibility.This work can provide a reference for the quality control of Compound Indigowoad Root Granule.

大青叶正丁醇提取物化学成分的HPLC/ESI-MSn研究

High performance liquid chromatography-electrospray ionization mass spectrometry(HPLC/ESI-MSn) was applied to analyze the chemical constituents from n-BuOH extract of Folium Isatidis.The data of retention time,UV spectra,molar masses and structural information on the compounds were obtained.Seventeen compounds are found in extract from n-BuOH.There are four nucleosides,two purines and eleven flavones.

ESI-MS法研究白芍炮制前后化学成分的变化

ESI-MS analytical method was employed to study extracts of unprocessed and processed Radix Paeoniae alba.The results of the experiments prove that different processed methods is making a certain different influence on the contents of chemiacl components in Radix Paeoniae alba.This method is simple and accurate.It can be used for analyse of Traditional Chinese Medicine(TCM).

乌头碱在家兔肠道内代谢产物的LC/ESI-MSn研究

采用LC/ESI-MSn的方法对家兔肠道内的乌头碱代谢产物进行研究,经与空白组比较发现,给药后家兔小肠内容物中新增加6个化合物峰(M1～M6),盲肠内容物中新增加5个化合物峰(M2～M6),粪便中新增加2个化合物峰(M3、M4). 分别测定各化合物的准分子离子及各级串联碎片离子,并与标准品的质谱断裂规律进行比较,同时参考文献,推断肠道内化合物M1为16-O-去甲基-8-O-去乙酰基乌头碱,M2为8-O-去乙酰基乌头碱,M3为16-O-去甲基乌头碱,M4为乌头碱(AC),M5为去氧乌头碱,为印乌头碱。

Bimolecular quadruplexes and their transitions to higher-order molecular structures detected by ESI-FTICR-MS

Four individual quadruplexes, which are self-assembled in ammonium acetate solution from telomeric sequences of closely related DNA strands - d(G(4)T(4)G(4)), d(G(3)T(4)G(4)), d(G(3)T(4)G(3)), and d(G(4)T(4)G(3)) - have been detected in the gas phase using electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS). The bimolecular quadruplexes associate with the same number of NH4+ in the gas phase as NMR shows that they do in solution. The quadruplex structures formed in solution are maintained in the gas phase. Furthermore, the mass spectra show that the bimolecular quadruplexes generated by the strands d(G(3)T(4)G(3)) and d(G(4)T(4)G(3)) are unstable, being converted into trimolecular and tetramolecular structures with increasing concentrations of NH4+ in the solution. Circular dichroism (CD) spectra reveal structural changes during the process of strand stoichiometric transitions, in which the relative orientation of strands in the quadruplexes changes from an antiparallel to a parallel arrangement. Such changes were observed for the strand d(G(4)T(4)G(3)), but not for the strand d(G(3)T(4)G(3)). The present work provides a significant insight into the formation of various DNA quadruplexes, especially the higher-order species.

Studies on the content variation of chemical constituents during the combination of ginseng with veratrum nigrum by ESI-MS and HPLC-ESI-MS

To study the content variation of ginsenosides and alkaloids during combination of ginseng with veratrum nigrum, the ginsenosides and alkaloids in the decoction of ginseng with veratrum nigrum were analyzed and compared by high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and electrospray ionization-mass spectrometry (ESI-MS). In the compatible decoction, eight ginsenosides and eight alkaloids. were detected, and the contents of six ginsenosides were found to be reduced, on the contrary, the contents of six alkaloids were increased. During combination of ginseng with veratrum nigrum, the contents of ginsenosides were reduced and those of the toxic alkaloids were increased. From the chemical point of view, the traditional theory is right that ginseng and veratrum nigrum are incompatible with each other.