太谷县图书馆藏两种银谱概略

本文介绍了太谷县图书馆馆藏清光绪十七年(1891)和咸丰十一年(1861)两种银谱手抄本,即《银谱便览》《银谱》的独特之处;分析了银谱类著作出现的历史原因,即商品经济的发展繁荣导致商业类实用书增多,银锭的自由铸造使得各地银锭的名称和成色各异,对银锭成色的鉴定显得尤为重要,而太谷作为晋商故里,商业繁荣,票号银号钱庄林立,银谱一类著作应用广泛;最后论述了研究银谱类著作的现实意义,指出公共图书馆在传承、保护、研究和利用优秀的传统文献资源等方面应发挥相应作用。

High Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometric Analysis of Bilobalide and Ginkgolides in Ginkgo biloba L. Leaves

The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.

Study and Application of Fingerprints of Ginkgo biloba Leaves Preparations

Aim To establish a method for determination of Ginkgo biloba L, its extractand preparations with HPLC fingerprints, so as to control the quality of the preparations. MethodsHPLC-DAD method was used to determine the constituents in preparations. Diamonsil? C_(18) (200mm X 4.6 mm, 5 μm) was used as analytical column, and acetonitrile/KH_2PO_4 was used as mobilephase with gradient elu-tion. The column temperature was at 24 ℃. The HPLC profile of chemicalconstituents of control sample and preparations were analyzed using similarity software. Results Thefingerprints of different preparations from different companies were slightly different because ofthe different preparing procedures. Mean while, the fingerprints of different batches of the samepreparation from the same company were similar to each other and the technology of each preparationwas stable. Conclusion This method is accurate, reproducible , simple, and can be used as ananalytical method for the routine quality control of Ginkgo biloba preparations.

Analysis of Volatile Constituents in Lonicera japonica Thunb. from Different Origins by GC-MS

[Objective] This study aimed to analyze the volatile constituents in Lonicera japonica Thunb. from different origins. [Method] HP-5MS capillary columns were used and column temperature was controlled by a program. MS analysis was performed with EI and quadruple mass analyzer. The volatile constituents in L. japonica Thunb. were identified by NIST02 and Wiley275 libraries, and their relative contents were determined with chromatographic peak area normalization method. [Result] According to GC-MS total ion-current chromatograms, 35 volatile constituents were identified in L. japonica Thunb. from Guangxi Zhuang Autonomous Region, mainly including methyl linolenate, n-hexadecanoic acid and ζ-muurolene; 18 volatile constituents were identified in L. japonica Thunb. from Hunan Province, mainly including n-hexadecanoic acid, linoleic acid and α-curcumene. [Conclusion] Main volatile constituents in L. japonica Thunb. from two different origins varied significantly.

Isolation and Preparative Purification for Ginkgolides A and B

In this paper a simple preparative method for isolation and purification of ginkgolides A and B was developed,As starting material,a commercially available standardized ginkgo extract (EGb761,containing 24% flavonoid and 6% terpene trilactones) was used,After a pretreatment step,optimized by the uniform design method ,the concentrated intermediate extract with high content of GA and gb(+90%) was separated into the individual terpenes by preparative liquid chromatography eluted with petroleum ether-ethylacetate,Analysis of products was carried out by means of HPLC-ELSD(evaporative light -scattering detector),The results show that ginkgolides A and B are obtained in higher yield and better purity.

Role of copper in tarnishing process of silver alloys in sulphide media

Silver and silver alloys usually tarnish,which causes some changes in their aesthetic appearance and electrical properties,due to their exposure to sulphide environments(H2S),and this is a problem in the field of corrosion and conservation of cultural heritage metallic artefacts.In this study,the role of copper content in the tarnishing process of 0.925,0.800 and 0.720 silver alloys in a 0.07 vol.%ammonium sulphide solution for different immersion periods was analyzed by electrochemical impedance spectroscopy(EIS)and scanning electron microscopy(SEM).The polarisation curves showed that the copper content and sulphide increased the corrosion current density and delayed the passivation of silver alloys.The impedance spectra collected at the open circuit potential(OCP)showed a single capacitive,incomplete and depressed loop,indicating that the charge transfer resistance decreased as the copper content increased in the alloys.In contrast,the double-layer capacitance increased as the copper content increased.The SEM-EDS analysis confirmed that the copper-rich phase in the silver alloys was selectively dissolved due to the preference of S to react with Cu,resulting in a localised attack,thus delaying the formation of a passive film.A marked localised attack was observed in alloys with lower copper content.The mechanism for the tarnishing of silver alloys in sulphide media was dependent on the nature of the alloy and the greater affinity of copper for sulphur.The dissolution of Ag and Cu to form corrosion products was proposed as the rate determining step.

Highly Sensitive Silver Nanorod Arrays for Rapid Surface Enhanced Raman Scattering Detection of Acetamiprid Pesticides

The determination of pesticide residue on agricultural products is increasingly important. Exposure to pesticides can cause severe acute reactions in humans, including aplastic anemia and leukemia. In this work, we developed a rapid and sensitive method to detect acetamiprid pesticide residue based on surface-enhanced Raman scattering. Silver nanorod （AgNR） arrays were fabricated by oblique angle deposition technology and were used as SERS substrates. Prior to detection, the AgNR arrays were cleaned with nitric acid solution or a mixture of methanol and acetone. Compared to the unwashed AgNR arrays, the AgNR arrays washed with methanol and acetone shows a signal enhancement 1000 times greater than the unwashed AgNR array due to the effective removal of the impurities on its surface. The limit of detection of acetamiprid was determined to be 0.05 mg/L. In addition, the molecular structure of acetamiprid was simulated and the corresponding vibration modes of the characteristic bands of acetamiprid were calculated by density function theory. To demonstrate its practical application, the AgNRs array substrates were applied successfully to the rapid identification of acetamiprid residue on a cucumber＇s surface. These results confirmed possibility of utilizing the AgNRs SERS substrates as a new method for highly sensitive pesticide residue detection.

Exploring the Interactions of Atomic Oxygen on Silver Clusters with Hydrogen

The interactions between AgnO- （n=1-8） and H2 （or D2） were explored by combination of the mass spectroscopy experiments and density function theory （DFT） calculations. The experiments found that all oxygen atoms in AgnO- （n--1-8） are inert in the interactions with H2 or D2 at the low temperature of 150 K, which is in contrast to their high reactivity with CO under the same condition. These observations are parallel with the preferential oxidation （PROX） of CO in excess hydrogen catalyzed by dispersed silver species in the condensed phase. Possible reaction paths between AgnO- （n=1-8） and H2 were explored using DFT calculations. The results indicated that adsorption of H2 on any site of AgnO- （n=1-8） is extremely weak, and oxidation of H2 by any kind of oxygen in AgnO- （n=1-8） has an apparent barrier strongly dependent on the adsorption style of the ＂O＂. These experiments and theoretical results about cluster reactions provided molecule-level insights into the activity of atomic oxygen on real silver catalysts.

Synthesis and Structural Characterizations of the Heteronuclear Cubane-like Cluster W_2Ag_2S_4(tdt)_2(PPh_3)_2·CH_2Cl_2

A new heterometallic cluster W2Ag2S4(tdt)2(PPh3)2·CH2Cl2(H2tdt=H2CH3C6H3S2)(Ⅱ) has been prepared from the reaction of a well-defined molecular building block W2S4(tdt)22-(I) with Ag complex. The compound has been characterized by X-ray diffraction study, IR., UV-Vis Spectroscopy and cyclic voltammetry.Crystallographic data for the compound are: space group P21/n,a=17.234(4), b=17.622(4), c=19. 094(4) A,β= 99. 22(2)°,V=5704(2) A3, Z=4,final R=0. 042 and Rw=0. 049 for 5983 independent reflections with I≥3σ(I) The structure analysis reveals that the cluster contains a cubane-like core [W2Ag2S4]4+ . The coordination geometry of each tungsten atom is a square pyramid just as that in the building block. Two types of metal-metal bonds of W-W bond and W-Ag bond exist in the core. The distance between two Ag atoms is out of the range of bonding.

Polyacrylic acid sodium salt film entrapped Ag-nanocubes as molecule traps for SERS detection

Surface-enhanced Raman spectroscopy （SERS） is a fast analytical technique for trace chemicals; however, it requires the active SERS-substrates to adsorb analytes, thus limiting target species to those with the desired affinity for substrates. Here we present networked polyacrylic acid sodium salt （PAAS） film entrapped Ag-nanocubes （denoted as Ag-nanocubes@PAAS） as an effective SERS-substrate for analytes with and without high affinity. Once the analyte aqueous solution is cast on the dry Ag-nanocubes@PAAS substrate, the bibulous PAAS becomes swollen forcing the Ag-nanocubes loose, while the analytes diffuse in the interstices among the Ag-nanocubes. When dried, the PAAS shrinks and pulls the Ag-nanocubes back to their previous aggregated state, while the PAAS network ＂detains＂ the analytes in the small gaps between the Ag-nanocubes for SERS detection. The strategy has been proven effective for not only single- analytes but also multi-analytes without strong affinity for Ag, showing its potential in SERS-based simultaneous multi-analyte detection of both adsorbable and non-adsorbable pollutants in the environment.

Alumina-coated Ag nanocrystal monolayers as surfaceenhanced Raman spectroscopy platforms for the direct spectroscopic detection of water splitting reaction intermediates

A novel Ag-alumina hybrid surface-enhanced Raman spectroscopy （SERS） platform has been designed for the spectroscopic detection of surface reactions in the steady state. Single crystalline and faceted silver （Ag） nanoparticles with strong light scattering were prepared in large quantity, which enables their reproducible self-assembly into large scale monolayers of Raman sensor arrays by the Langrnuir-Blodgett technique. The close packed sensor film contains high density of sub-nm gaps between sharp edges of Ag nanoparticles, which created large local electromagnetic fields that serve as ＂hot spots＂ for SERS enhancement. The SERS substrate was then coated with a thin layer of alumina by atomic layer deposition to prevent charge transfer between Ag and the reaction system. The photocatalytic water splitting reaction on a monolayer of anatase TiO2 nanoplates decorated with Pt co-catalyst nanoparticles was employed as a model reaction system. Reaction intermediates of water photooxidation were observed at the TiO2/solution interface under UV irradiation. The surface-enhanced Raman vibrations corresponding to peroxo, hydroperoxo and hydroxo surface intermediate species were observed on the TiO2 surface, suggesting that the photo-oxidation of water on these anatase TiO2 nanosheets may be initiated by a nucleophilic attack mechanism.

Superionic conductor-mediated growth of ternary ZnCdS nanorods over a wide composition range

Composition regulation of semiconductors can engineer their bandgaps and hence tune their properties. Herein, we report the first synthesis of ternary ZnxCd1-xS semiconductor nanorods by superionic conductor （AgRS）-mediated growth with [（C4H9）2NCS2]2M （M = Zn, ca） as single-source precursors. The compositions of the ZnKCd1-xS nanorods are conveniently tuned over a wide range by adjusting the molar ratio of the corresponding precursors, leading to tunable bandgaps and hence the progressive evolution of the light absorption and photoluminescence spectra. The nanorods present well-distributed size and length, which are controlled by the uniform Ag2S nanoparticles and the fixed amount of the precursors. The results suggest the great potential of superionic conductor-mediated growth in composition regulation and bandgap engineering of chalcogenide nanowires/nanorods.

Citric acid-assisted synthesis of nano-Ag/BiO Br with enhanced photocatalytic activity

In this study, silver nano-particles have been anchored in the surface of Bi OBr photocatalysts by a citric acid-assisted photoreduction method. The citric acid was served as a chelating and reductive agent for the preparation of Ag-decorated Bi OBr photocatalysts(named as Ag/Bi OBr-2). The as-synthesized samples were characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), scanning electron microscopy(SEM), transmission electron microscopy(TEM), and UV-Vis diffuse reflection spectroscopy(DRS). The Ag/Bi OBr-2 photocatalyst exhibited excellent and stable photocatalytic activities on MO and phenol degradation under simulated sunlight irradiation. The enhanced photocatalytic activity could be ascribed to the smaller size, rough surface, and the surface plasma resonance(SPR) effect of Ag. Also, the Schottky junction, between the surface of the Bi OBr and silver nanoparticles, accelerated the efficient transfer and separation of photoinduced electron-hole pairs and promoted the photocatalytic performance. The active species tests indicated that the superoxide radical(·O-2) was responsible for the enhanced photocatalytic performance of Ag/Bi OBr-2. Finally, a possible photocatalytic mechanism was proposed.

Optical response and SERS properties of individual large scale supracrystals made of small silver nanocrystals

There is a considerable interest in producing and understanding the optical and spectroscopic properties of ordered nanoparticle assemblies. Herein, we describe and interpret the optical absorbance and Raman properties of 5.9 nm ± 0.3 nm diameter silver nanocrystals coated with dodecanethiol and organized in highly ordered 3D superlattices of different heights. Each superlattice was studied individually, which allowed to elaborate a model based on Maxwell-Garnett theory to reproduce qualitatively the height and wavelength dependence of the absorbance. Importantly, because of their small size compared to that of traditional nanoparticles used in Surface Enhanced Raman Spectroscopy （SERS）, the large 3D distribution of hot spots generated by the silver superlattices allowed to easily obtain SERS spectra of the surrounding ligands despite their intrinsic low Raman cross section. Accordingly, traces of thiophenol could be detected very easily.

Simultaneous determination by UPLC-MS/MS of seven bioactive compounds in rat plasma after oral administration of Ginkgo biloba tablets: application to a pharmacokinetic study

A rapid, reliable, and sensitive method was developed using ultra-performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS） with an electrospray ionization （ESI） source for determination of seven bioactive compounds in rat plasma after oral administration of Ginkgo biloba tablets （GBTs）. The method simultane- ously detects bilobalide （BB）, ginkgolide A （GA）, ginkgolide B （GB）, ginkgolide C （GC）, quercetin （QCT）, kaempferol （KMF）, and isorhamnetin （ISR） for pharmacokinetic study. The analytes and internal standard （IS） were extracted from rat plasma by acetidin. An MS/MS detection was conducted using multiple reaction monitoring （MRM） and operating in the negative ionization mode. The calibration curve ranges were 5-500, 5-500, 2.5-250, 1-100, 1-100, 1-100, and 1-100 ng/ml for BB, GA, GB, GC, QCT, KMF, and ISR, respectively. The mean recovery of the analytes ranged from 68.11% to 84.42%. The intra- and inter-day precisions were in the range of 2.33%-9.86% and the accuracies were between 87.67% and 108.37%. The method was used successfully in a pharmacokinetic study of GBTs. The phar- macokinetic parameters of seven compounds were analyzed using a non-compartment model. Plasma concentrations of the seven compounds were determined up to 48 h after administration, and their pharmacokinetic parameters were in agreement with previous studies.

Chemical interactions between silver nanoparticles and thiols: a comparison of mercaptohexanol against cysteine

The interaction between citrate capped silver nanoparticles and two different thiols, mercaptohexanol （MH） and cysteine, was investigated. The thiols interacted with silver nanoparticles in a significantly contrasting manner. With MH, a sparingly soluble silver（1） thiolate complex AgSRm （Rm = -（CH2）6OH） was formed on the silver nanoparticle surface. Cyclic voltammograms and UV-vis spectra were used to infer that the AgSRm complex on the nanoparticle surface undergoes a phase transition to give a mixture of AgSRm and Ag2S-like complexes. In contrast, when silver nanoparticles were exposed to cysteine, the citrate cap- ping agent on the silver nanoparticles was replaced by cysteine to give cysteine capped nanoparticles. As cysteine capped nanoparticles form, the electrochemical data displayed a decrease in oxidative peak charge but the UV-vis spectra showed a constant signal. Therefore, cysteine capped nanoparticles were suggested to have either inactivated the silver surface or else pro- moted detachment from the electrode surface.