Study on the variation of chemical constituents during combination of ginseng with trogopteroum feces and semen raphani by high performance liquid chromatography-mass spectrometry

A high performance liquid chroatography-electrospray ionization-mass spectrometric method was developed for analysis and identification of ginsenosides from the decoction of ginseng, ginseng with trogopteroum feces and ginseng with semen raphani. Ten ginsenosides were separated and detected. The content variation of these ginsenosides was researched. The experimental results showed, that ginsenosides were less in compatible decoction than in separate one expect Ro. the stripping of ginsenosides were restrained by semen raphani and during combination of ginseng with trogopteroum feces, the precipitates were produced by ginsenosides.

Studies on the flavones using liquid chromatography-electrospray ionization tandem mass spectrometry

Fragmentation pathways of nine flavone compounds have been studied by using electrospray ionization multi-stage tandem mass spectrometry (ESI-MSn). Analyzing the product ion spectra of flavonoids and aglycones, we observed some diagnostic neutral losses, such as *CH3, H2O, residue of glucose and gluconic acid, which are very useful for the identification of the functional groups in the structures. Furthermore, specific retro Diels-Alder (RDA) fragments for flavones with different hydroxyl substitution have also been discussed. The information is helpful for the rapid identification of the location site of hydroxyl substitution on flavones. Fragmentation pathways of C-glycosidic flavonoid have also been discussed using ESI-MSn, demonstrating ions [M-H-60](-), [M-H-90](-), [M-H-120](-) are characteristic ions of C-glycosidic flavonoid. According to the fragmentation mechanism of mass spectrometry and HPLC-MS data, the structures of seven flavones in Scutellaria baicalensis Georgi have been identified on-line without time-consuming isolation. The HPLC-ESI-MSn method for analyzing constituents in the Scutellaria baicalensis Georgi has been established.

Hydrodynamic radius characterization of a vinyl-type polynorbornene by size-exclusion chromatography with a static and dynamic laser light scattering detector

Both absolute molecular weight and molecular sizes (radius of gyration and hydrodynamic radius) of a vinyl-type polynorbornene eluting from size-exclusion chromatography columns were determined by combined with a static and dynamic laser light scattering detector. The hydrodynamic radius of polymer fraction eluting from size-exclusion chromatography columns was obtained from dynamic laser light scattering measurements at only a single angle of 900 by introducing a correction factor. According to the scaling relationship between molecular sizes and molecular weight and the ratio between radius of gyration and hydrodynamic radius, the vinyl-type polynorbornene took a random coil conformation in 1,2,4-trichlorobenzene at 150 degreesC.

Studies of instrumental spreading in gel permeation chromatography by coupling with a two-angle laser light scattering detector

The instrumental spreading of a high temperature gel permeation chromatograph (GPC) was evaluated by coupling with a two-angle laser light scattering (TALLS) detector, using narrow polystyrene, polyethylene, and syndiotactic polypropylene samples. The determined spreading factor increased with increasing molecular weight of polymers, and no maximum for spreading 174 tor was observed in the studied retention volume, while the spreading factors for single low molecular weight alkanes are independent of their molecular weight. Neglecting of the spreading effect for GPC would not introduce much error in molecular weight calculation when high quality high performance columns were used, especially when equipped with a laser light scattering detector. The scaling relationship between radius of gyration and molecular weight of polymer, determined by GPC with a TALLS detector, was independent of the instrumental spreading.

A new method of measuring alcohol clusters in polyimide membrane: combination of inverse gas chromatography with equilibrium swelling

A new method of measuring the mean size of solvent clusters in swollen polymer membrane is presented in this paper. This method is based on a combination of inverse gas chromatography (IGC) and equilibrium swelling. The mechanism is that weight fraction activity coefficient of solvent in swollen polymer is influenced by its clusters size. The mean clusters size of solvent in swollen polymer can be calculated as the quotient of the weight fraction activity coefficient of clustering system dividing the weigh fraction activity coefficient of non-clustering system. In this experiment, the weigh fraction activity coefficient of non-clustering system was measured with IGC. Methanol, ethanol and polyimide systems were tested with the new method at three temperatures, 20, 40, and 60degreesC. The mean clusters size of methanol in polyimide was five, four, and three at each temperature condition, respectively. Ethanol did not form clusters (the mean clusters size was one). In contrast to the inherent narrow temperature range in DSC, XRD, and FTIR methods, the temperature range in IGC and equilibrium swelling is broad. Compared with DSC. XRD. and FTIR, this new method can detect the clusters of solvent-polymer system at higher temperature.

Determination of molecular weight and molecular sizes of polymers by high temperature gel permeation chromatography with a static and dynamic laser light scattering detector

Flow-mode static and dynamic laser light scattering (SLS/DLS) studies of polymers, including polystyrene, polyethylene, polypropylene and poly(dimethylsiloxane) (PDMS), in 1,2,4-trichlorobenzene (TCB) at 150 degreesC were performed on a high temperature gel permeation chromatography (GPC) coupled with a SLS/DLS detector. Both absolute molecular weight (M) and molecular sizes (radius of gyration, R-g and hydrodynamic radius, R-h) of polymers eluting from the GPC columns were obtained simultaneously. The conformation of different polymers in TCB at 150 degreesC were discussed according to the scaling relationships between R-g, R-h and M and the rho-ratio (p = R-g/R-h). Flow-mode DLS results of PDMS were verified by batch-mode DLS study of the same sample. The presented technique was proved to be a convenient and quick method to study the shape and conformation of polymers in solution at high temperature. However, the flow-mode DLS was only applicable for high molecular weight polymers with a higher refractive index increment such as PDMS.

Separation of scandium, yttrium and lanthanum in high-performance centrifugal partition chromatography with S-octyl phenyloxy acetic acid

Separation of scandium(III), yttrium(III) and lanthanum(III) was performed by high-performance centrifugal partition chromatography (HPCPC) employing the stationary phase of S-octyl phenyloxy acetic acid (CA-12). The liquid-liquid extraction behavior of CA-12 for Sc(III), Y(III) and La(III), the acidity of aqueous phase, and the operation conditions of HPCPC were examined. The retention volume (V-R) increased with the order of Y(III), La(III) and Sc(III) accompanied with the elution of the mobile phase in different pH, which is lowered from 4.6 to 2.1.

Analysis of chemical constituents of essential oil in purple magnolia leaves by gas chromatography-mass spectrometry

The essential oil in purple magnolia leaves was extracted by steam distillation approaches. The oil obtained was dried with anhydrous magnesium sulfate. According to the analysis of gas chromatography/mass spectrometry, more than 40 peaks were separated and 32 compounds were identified. The identified constituents represent 95% of the peak area of the essential oil. The main compounds were germacrene-D, santolina triene, caryophyllene, 1,3,7-octatriene, 3,7-dimethyl, and camphene, etc.

Rapid identification of saponins in plant extracts by electrospray ionization multi-stage tandem mass spectrometry and liquid chromatography/tandem mass spectrometry

Electrospray ionization multi-stage tandem mass spectrometry (ESI-MSn) and liquid chromatography coupled with on-line mass spectrometry (LC/MS/MS) were applied to characterize saponins in crude extracts from Panax ginseng. The MSn data of the [M - H](-) ions of saponins can provide structural information on the sugar sequences of the saccharide chains and on the sapogins of saponins. By ESI-MSn, non-isomeric saponins and isomeric saponins with different aglycones can be determined rapidly in plant extracts. LC/MS/MS is a good complementary analytical tool for determination of isomeric saponins. These approaches constitute powerful analytical tools far rapid screening and structural assignment of saponins in plant extracts. Copyright (C) 2000 John Wiley & Sons, Ltd.

Quantitative structure-property relationship research to the analysis of photoionization sensitivity of organic compounds in gas chromatography

The A(m) index and molecular connectivity index were used for studying the photoionization sensitivity of some organic compounds in gas chromatography. The analysis of structure-property relationship between the photoionization sensitivity of the compounds and the A(m) indices or molecular connectivity indices has been carried out. The genetic algorighm was used to build the correlation model in this field. The results demonstrate that the property of compounds can be described by both A(m) indices and molecular connectivity indices, and the mathematical model obtained by the genetic algorithm was better than that by multivariate regression analysis.

The research of cellulose derivatives as chiral stationary phases and high performance liquid chromatography with polarimeter as on-line detector

Three cellulose derivatives were synthesized and used as chiral stationary phases based on silica gel. The effects of adsorbances on the column numbers and stabilities have been investigated. These stationary phases exhibited high chiral recognition for various racemates. At the same time, the on-line curves of polarimeter were obtained by high performance liquid chromatography with polarimeter as on-line detector.

Determination of 14 rare earth impurities in Y2O3 by petroleum sulfoxide extraction chromatography

Petroleum sulfoxide-NH4SCN extraction chromatography was developed for the separation of Y from other rare earth elements. Some chromatographic parameters were chosen and separation factors between Y and other rare earth elements were determined. A column of resin coated with petroleum sulfoxide was used. The Y in the sample was eluted with NH4SCN, then titrated with EDTA. The recovery was 67%-120% and relative standard deviation +/-4.0%-19.4%. This method can be applied to the determination of trace amounts of rare earth impurities in Y2O3 with a purity of 99.999 9%-99. 999 99%.

Determination of rare-earth impurities in ultra-highly pure Er2O3 and Ho2O3 by [HEH(HEP)] extraction chromatography-atomic emission spectrometry

This article applied [HEH(HEP)] (2-ethyhexyldrogen-2-ethylhexyl phosphonate)extraction chromatography to separate 14 rare earth impurities from ultra-highly pure Er2O3 and Ho2O3, and then the impurities were determined by atomic emission spectrometry. The average percentage recovery for each element is in the range of 70%similar to 140%. The relative standard deviations of the determination are +/-3.3%similar to 2.2%. This method can be applied to the determination of the trace amounts of rare eath impurities in Er2O3 and Ho2O3 with a purity of 99.999 9%-99.999 99%.

Electrospray ionization mass spectrometry of cyclodextrin complexes with amino acids in incubated solutions and in eluates of gel permeation chromatography

1:1 complexes of beta-cyclodextrin (CD) with three amino acids (Gly, Phe and Trp) have been detected as ions in the gas phase using infusion positive and negative ion electrospray ionization mass spectrometry (ESI-MS). In contrast with the positive ion ESI mass spectra of simple aqueous solutions, the aggregates and adducts usually formed in the ESI process did not appear in the positive ion ESI spectra of solutions buffered with ammonium acetate (NH4Ac), even at higher analyte concentrations, These studies suggest that addition of buffer and/or use of a low analyte concentration should be used to overcome formation of aggregates and metal ion adducts in such mass spectrometry studies. Also, the deprotonated complexes are dissociated by collision induced dissociation (CID) to form an abundant product ion, the deprotonated CD, requiring transfer of a proton to the amino acid carboxyl group, To understand formation of complexes in the gas phase, gel permeation chromatography (GPC) was used to separate free amino acids (AAs) from complexes in an incubated solution. The ESI mass spectra of the GPC fractions show the presence of 1:1 complexes of both CD-aromatic amino acids and CD-aliphatic amino acids. Compared with CD-aliphatic amino acid complexes, CD-aromatic amino acid complexes appear to be destabilized in the gas phase, possibly because the hydrophobic interaction which binds the aromatic group of amino acids in the CD cavity in solution may become repulsive when solvent evaporates from the droplets during the electrospray process, whereas those complex ions formed as proton bound dimers are stabilized by electrostatic forces, the major binding force for such complexes in the gas phase. In addition, the GPC technique coupled with off-line ESI-MS can rapidly separate CD complexes by size, and provides some information on the character of the complexes in solution. (C) 1998 John Wiley & Sons, Ltd.