Silver complexation and tandem mass spectrometry for differentiation of triterpenoid saponins from the roots of Pulsatilla chinensis (Bunge) Regel.
For detection and differentiation of two types of triterpenoid saponins based on different aglycons of the lupane and oleanane skeleton from the roots of Pulsatilla chinensis (Bunge) Regel, the silver ion was introduced and electrospray ionization multi-stage tandem mass spectrometry was applied to analyze eleven triterpenoid saponin silver complexes. The quasi-molecular ion [M+Ag](+) was observed in the full-scan MS spectra of all the silver complexes. The MS(2) data of the [M+Ag](+) ion provided structural information on the sugar sequence of the oligosaccharide chains and the aglycon of the saponins. There are two patterns in the cleavage pathway of oleanane-type saponins. One is elimination of the sugar chain and subsequent loss of the carboxylic group which is the same as the cleavage of lupine-type saponins. The other is loss of the distinguishing ions at m/z 72 and 28 (C(2)H(4)) followed by loss of the carboxylic group. Diagnostic fragmentation pathways of the silver complexes of the saponins allow successful identification of the two types of saponins from the roots of Pulsatilla chinensis (Bunge) Regel.
Development of a novel method for triterpenoidal saponins in rat plasma by solid-phase extraction and high-performance liquid chromatography tandem mass spectrometry.
A novel method using high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been developed for the quantification of four triterpenoidal saponins (anemoside B4, pulsatilloside B, anemoside A3, and 23-hydroxybetulinic acid) in rat plasma following solid-phase extraction (SPE). The optimized procedure utilized off-line extraction of the analytes from plasma using polymeric (Strata-X) SPE cartridges. Detection and quantitation were performed by MS/MS using electrospray ionization (ESI) and multiple reaction monitoring (MRM) in a novel multiswitching monitoring mode. The analytes and internal standard (scutellarin) were analyzed using a Sapphire C18 column (250×4.6 mm, 5 μm) with a linear gradient elution. The mass transition ion pairs of the triterpenoidal saponins were executed as follows: m/z 1219.7/749.4 for anemoside B4, m/z 819.4/347.2 for pulsatilloside B, m/z 749.6/471.2 for anemoside A3, m/z 471.4/471.4 for 23-hydroxybetulinic acid, and m/z 461.1/285.0 for the internal standard. The specificity, linearity, accuracy, precision, recovery, matrix effect, and stabilities were validated for all analytes in the plasma samples. In conclusion, the validation results demonstrate that this method is robust and specific. This validated method is a novel technique for sample preparation and quantitation and was successfully applied to estimate the pharmacokinetics of triterpenoidal saponins.
Heat Transfer Characteristic for a New Plate Metal Hydride Reactor
The property of major metal hydride reactors in the world was analyzed and a new plate metal hydride reactor was designed.An experimental facility to test the metal hydride reactor was also designed correspondingly.The effective thermal conductivity of the plate metal hydride reactor was measured by varying the initial metal hydride packing fraction,the kind of filled gas and the pressure of the filled gas,cycle numbers.The test results show that the effective thermal conductivity of the reactor,has exceeded(7.5) W/(m·K) before activation,which is increased greatly.After alloy activation,the effective thermal conductivity of the reactor has a linear change trend with the hydrogen pressure during the interval 0.1~3.5 MPa.The effective thermal conductivity of the reactor just only decreases quickly at the beginning,but becomes stable after several cycles.