HL—1装置碳化和采用抽气孔栏时的可见辐射观测

本文描述了HL-1装置器壁碳化和采用抽气孔栏时,氢及杂质通量的变化情况;利用多道可见辐射的时空分布测量,得到了MARFE放电,在产生MARFE时,辐射热也相应增强。     

Efficient Gating of Ion Transport in Three‐Dimensional Metal–Organic Framework Sub‐Nanochannels with Confined Light‐Responsive Azobenzene Molecules

1D nanochannels modified with responsive molecules are fabricated to replicate gating functionalities of biological ion channels, but gating effects are usually weak because small molecular gates cannot efficiently block the large channels in the closed states. Now, 3D metal–organic framework (MOF) sub‐nanochannels (SNCs) confined with azobenzene (AZO) molecules achieve efficient light‐gating functionalities. The 3D MOFSNCs consisting of a MOF UiO66 with ca. 9–12 Å cavities connected by ca. 6 Å triangular windows work as angstrom‐scale ion channels, while confined AZO within the MOF cavities function as light‐driven molecular gates to efficiently regulate the ion flux. The AZO‐MOFSNCs show good cyclic gating performance and high on–off ratios up to 17.8, an order of magnitude higher than ratios observed in conventional 1D AZO‐modified nanochannels (1.3–1.5). This work provides a strategy to develop highly efficient switchable ion channels based on 3D porous MOFs and small responsive molecules.     

Systematic screening and characterization of novel bufadienolides from toad skin using ultra‐performance liquid chromatography/electrospray ionization quadrupole time‐of‐flight mass spectrometry

During the discovery process of novel compounds, it is of significant importance to differentiate novel from known compounds in crude extracts before starting the time‐consuming process of purification. Bufadienolides are the main active components of the skin of the toad Bufo bufo gargarizans Cantor (toad skin), an important traditional Chinese medicine. The fragmentation behavior and mass spectra profiles of bufadienolides standards were investigated using ultra‐performance liquid chromatography/electrospray ionization quadrupole time‐of‐flight mass spectrometry (UPLC/ESI‐Q‐TOFMS). Several fragmentation rules were summarized and applied to characterize novel and known bufadienolides in toad skin. Characteristic substituent groups could be identified by both diagnostic ions and their relative abundance. Bufadienolide stereoisomers could be differentiated from positional isomers by comparing fragment abundance profiles. This was used to characterize new stereoisomers for known bufadienolides. A total of 39 bufadienolides were screened out using a systematic method developed in our laboratory. In addition to 19 known bufadienolides, 20 putative novel compounds, including 8 stereoisomers, were characterized. UPLC/Q‐TOFMS was demonstrated to be a powerful tool for the characterization of low‐abundance bufadienolides in complex samples. This study provides guidelines for the targeted isolation of novel bufadienolides from natural products. Copyright © 2010 John Wiley & Sons, Ltd.     

Purification and preparation of compounds from an extract of Scutellaria barbata D. Don using preparative parallel high performance liquid chromatography

Preparative parallel high performance liquid chromatography combined with solvent partition and other pretreatments were adopted to separate and purify compounds from an extract of Scutellaria barbata D. Don. Mass-triggered fraction collection allowed the rapid and precise isolation of target compounds. Twelve compounds were isolated from the extract of S. barbata D. Don, their purity in area percent was determined by HPLC analysis, and the structures of seven compounds were further identified with HPLC/ESI-MS, (1)H NMR, and( 13)C NMR, among which 4-(3,4-dihydroxy-phenyl)-but-3-en-2-one, acacetin-7-diglucuronide, and luteolin-7-diglucuronide were the first to be identified from this plant. The results demonstrated that multi-channel parallel preparative HPLC/UV/MS is an efficient method for isolation and purification of compounds from natural products.     

A novel method of prediction and optimization for preparative high-performance liquid chromatography separation

The preparation of components from a complex sample is a difficult task. The optimization of the separation and subsequent scale-up is usually carried out by trial and error. In this study, the relationship between retention parameters a and c for analytical and preparative separations was developed when the same solid adsorbent and mobile phase were used. The prediction and optimization of the preparative separation of a complex sample could be achieved by direct and simple conversion of the experimentally determined data from an analytical level. The novel method was successfully applied to optimize the separation of target compounds in traditional Chinese medicine (TCM).     

High performance liquid chromatography-mass spectrometry analysis of protoberberine alkaloids in medicine herbs

RP-HPLC is the main method for the analysis of alkaloids. However, peak tailing is a problem that commonly occurs in the separation of alkaloids. In order to overcome this, three kinds of RP columns were compared for the analysis of protoberberine alkaloids in Coptidis Rhizoma and Phellodendri Cortex in this work. XTerra MS C18 column was the best one which gave the best symmetry factor under the same conditions. With this column, a good separation of the crude extracts of C. Rhizoma and P. Cortex was achieved using 0.1% v/v formic acid buffer and methanol as mobile phase. At the same time, the crude extracts of C. Rhizoma and P. Cortex were analyzed by the LC-ESI-MSn and LC-atmospheric pressure chemical ionization (APCI)-MSn methods. In the analysis of HPLC-ESI/MSn, structures of five protoberberine alkaloids were elucidated, compared to authentic standards, and data from the literature. At the same time, the structure of a novel compound was elucidated. In the HPLC-APCI/ MSn analysis, there was an interesting phenomenon that the relative abundance of the ions M+ and [M + 2]+ was different for different alkaloids. The possible fragmentation pathways of protoberberine alkaloids in APCI/MS analysis were studied for the first time in the present work.     

Studies of iridoid glycosides using liquid chromatography/electrospray ionization tandem mass spectrometry

Fragmentation pathways of five iridoid glycosides have been studied by using electrospray ionization multi-stage tandem mass spectrometry (ESI-MS(n)). The first-stage MS data of the five iridoid glycosides were compared. The MS spectra showed that the adduct ions of iridoid glycosides and the formate anion were diagnostic ions to distinguish iridoid glycosides with a carboxyl group at the C-4 position or an ester group at the C-4 position. The MS fragmentation pathways of the five iridoid glycosides were also studied. Analyzing the product ion spectra of iridoid glycosides, some neutral losses were observed, such as H(2)O, CO(2) and glucose residues, which were very useful for the identification of the functional groups in the structures of iridoid glycosides. Furthermore, specific loss of one molecule of methyl 3-oxopropanoate or 3-oxopropanic acid was firstly discussed, which corresponded to the isomerization of the hemiacetal group in the structure of iridoid aglycone. According to the fragmentation mechanisms and HPLC/MS(n) data, the structures of five iridoid glycosides in a crude extract of Gardenia jasminoisdes fruit have been identified. Three compounds were compared with standards and the other two were identified as shanzhiside and genipin gentibioside by their MS(n) data without standard compounds. In order to further validate the veracity of the deduction, genipin gentiobioside was isolated from the extract of Gardenia jasminoisdes fruit using Purification Factory and was further identified by C- and H-NMR.     

Radon transforms on Siegel-type nilpotent Lie groups

Let \mathfrak{N}:={{\displaystyle H}}_n\times {ℂ}^n be the Siegel-type nilpotent group, which can be identified as the Shilov boundary of Siegel domain of type II, where {{\displaystyle H}}_n denotes the set of all n\times n Hermitian matrices. In this article, we use singular convolution operators to define Radon transform on \mathfrak{N} and obtain the inversion formulas of Radon transforms. Moveover, we show that Radon transform on \mathfrak{N} is a unitary operator from Sobolev space W^n;2 into L²(\mathfrak{N}):     

The herbalome—an attempt to globalize Chinese herbal medicine

The herbalome is a project with the objective of globalizing Chinese herbal medicine (CHM) by clarification of its composition, structure, and function; by establishing a standard resource library; and by interpreting the synergistic and complementary mechanisms of multi-components on multi-targets. In phase I, it focuses on the development of systematic separation methodology for resolving and analyzing the complex components in CHM and establishment of a comprehensive resource library. This review summarizes recent advances in the herbalome project with regard to innovative separation techniques and demonstration of a resource library.