Characterization of saccharides and phenolic acids in the Chinese herb Tanshen by ESI-FT-ICR-MS and HPLC

This study sought to determine the main components (saccharides and phenolic acids) in crude extract of the Chinese herb Tanshen by electrospray ionization Fourier transform ion cyclotron resonant mass spectrometry (ESI-FT-ICR-MS) in negative-ion mode. Eleven compounds were identified as phenolic acids by exact mass measurement and further confirmed by sustained off-resonance irradiation (SORI) CID data. In addition, monosaccharicles and oligosaccharides (n = 2 similar to 5) and a serial of corresponding anionic adducts of saccharide were observed without adding any anions additionally to the extract solution, and the anionic components were unambiguously identified as H2O, HCl, HCOOH, HNO3, C3H6O2, H2SO4 and C5H7NO3 according to the exact mass measurement results.

Studies on the stability of diester-diterpenoid alkaloids from the genus Aconitum L. by high performance liquid chromatography combined with electrospray ionisation tandem mass spectrometry (HPLC/ESI/MSn)

The stability of diester-diterpenoid alkaloids (DDA) from plants of the genus Aconitum L. has been studied in different solvents and pH buffers. The HPLC/ESIMS method for analysing the concentration of DDA was established and DDA's decomposition products were elucidated by HPLC/ESI-MS/MSn. In different solvents, e.g. dichloromethane, ether, methanol and distilled water, the decomposition pathways of DDA are quite different and their difference in stabilities depends on the difference of their structures, in which substituents at the N atom and substituents at C-3 are different. The pyrolytic products of DDA, such as deacetoxy aconitine-type alkaloids, have been observed in the above solvents, whereas 8-methoxy-14-benzoyl aconitine-type alkaloids have been obtained only in methanol.

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。

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

Studies on the aconitine-type alkaloids in the roots of Aconitum Carmichaeli Debx. by HPLC/ESIMS/MSn

Studies of aconitine-type alkaloids in the Chinese herb Aconitum Carmichaeli were performed by HPLC/ESIMS/MSn and FTICR/ESIMS in positive ion mode. The characteristic fragmentation pathways in the MSn spectra were summarized based on previously published research literature and further study. According to the fragmentation pathways of mass spectrometry, results from the analysis of standard compounds and reports from literature, 111 compounds were identified or deduced in a total of 117 found compounds in A. Carmichaeli. In the 11 monoester-diterpenoid alkaloids (MDA), 10 diesterditerpenoid alkaloids (DDA) and 81 lipo-alkaloids, the novel alkaloids including 1 MDA, 2 DDA and 48 lipo-alkaloids were detected.

A quantitative HPLC method for determining lactide content using hydrolytic kinetics

A new method for quantitative analysis of lactide has been developed by applying chemical kinetics to a HPLC system. The most important advance is its practical approach to the quantification of analytes that are unstable in the HPLC mobile phase. In HPLC analysis, anhydrous mobile phases cannot separate lactide from impurities, and only mixtures of water and organic solvent can achieve effective separation. By selecting conditions for testing and studying the kinetics of lactide hydrolysis, extensive experiments revealed that lactide degradation can be treated as a pseudo-first-order reaction under the given HPLC conditions, and lactide content or purity can be quantitatively determined. This method is practical for measuring the purity of the intermediate lactide in polylactic acid (PLA) production and the lactide content in PLA.

Cinnamate-Functionalized Poly(ester-carbonate): Synthesis and Its UV Irradiation-Induced Photo-Crosslinking

A functionalized. cyclic carbonate monomer containing a cinnamate moiety, 5-methyl-5-cinnamoyloxymethyl-1,3-dioxan-2-one (MC), was prepared for the first time with 1,1,1-tri(hydroxymethyl) ethane as a starting material. Subsequent polymerization of the new cyclic carbonate and its copolymerization with L-lactide (LA) were successfully performed with diethyl zinc (ZnEt2) as initiator/catalyst. NMR was used for microstructure identification of the obtained monomer and copolymers. Differential scanning calorimetry (DSC) was used to characterize the functionalized poly(ester-carbonate). The results indicated that the copolymers displayed a single glass transition temperature (T-g) and the T, decreased with increasing carbonate content and followed the Fox equation, indicative of a random microstructure of the copolymer. The photo-crosslinking of the cinnamate-carrying copolymer was also demonstrated.

Undercut structures fabricated by microtransfer printing combined with UV exposure and their applications

In this paper. the undercut structures were fabricated by microtransfer printing of metal films on the surface of photoresist combined with UV exposure and photoresist film developing. The patterned metal films were used as mask to realize the selective UV exposure of photoresist Firstly. The undercut structures. which consist of the top metal films and the patterned bottom photoresist, formed in the subsequent developing process because of the lateral dissolving of photoresist at the edge of the unexposed regions. The method proposed in this paper has wider tolerance to the changing of the patterning parameters. but, without effect on patterning resolution since the metal film was used as the top layer. The undercut Structures were Used as separators to pattern passive-matrix display of organic light-emitting diodes (OLEDs). No visible difference of the device performance was observed Compared with the OLEDs patterned by the shadow mask.

Effects of ultrahigh pressure extraction conditions on yields and antioxidant activity of ginsenoside from ginseng

Ultrahigh pressure technique was employed to extract ginsenosides from roots of ginseng (Panax ginseng C.A. Meyer). The optimal conditions for ultrahigh pressure extraction (UPE) of total ginsenosides were quantified by UV-vis spectrophotometry with the ginsenoside Re as standard, the signal ginsenosides were quantified by HPLC and ELSD with ginsenosides Re, Rg(1), Rb-1, Rc and Rb-2 as standards. Orthogonal design was applied to evaluate the effects of four independent factors (extraction pressure, extraction temperature, extraction time and ethanol concentration) on the yield and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity of ginsenoside, which are based on microwave extraction (ME), ultrasound extraction (UE), soxhlet extraction (SE) and heat reflux extraction (HRE) method. The results showed that UPE method can produce ginsenoside with the highest yield and the best radical scavenging activity compared to other used ones. Scanning electron microscopic (SEM) images of the plant cells after ultrahigh pressure treatment was obtained to provide visual evidence of the disruption effect.

Type I collagen-mediated synthesis and assembly of UV-photoreduced gold nanoparticles and their application in surface-enhanced Raman scattering

We reported a simple method to synthesize gold nanoparticles (NPs) by photoreducing HAuCl4 in acetic acid solution in the presence of type I collagen. It was found that the collagen takes an important role in the formation of gold NPs. The introduction of collagen made the shape of the synthesized gold nanocrystals change from triangular and hexangular gold nanoplates to size-uniform NPs. On the other hand, thanks to the special characters of collagen molecules, such as its linear nanostructure, are positively charged when the pH < 7, and the excellent self-assembly ability, photoreduced gold NPs were assembled onto the collagen chains and formed gold NPs films and networks. A typical probe molecule, 4-aminothiophenol, was used to test the surface-enhanced Raman scattering activity of these gold NPs films and networks and the results indicated good Raman activity on these substrates.

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.