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    Influence of the Combustion Interface Using Auxiliary Gas on the Carbon Isotope Analysis of Organic Compounds
    JIA Wang-Lu, LIU Jin-Zhong, PENG Ping-An
    Chemical Journal of Chinese Universities    2012, 33 (04): 718-724.   DOI: 10.3969/j.issn.0251-0790.2012.04.014
    Abstract2583)      PDF(pc) (2292KB)(354)       Save
    Combustion reactor is considered to be one of the critical factors in detecting sensitivity and resolution of organic compounds for carbon isotope analysis, yet the reasons are not well understood. This study focused on combustion reactors using additional auxiliary gas, one of the two most commonly used reactors applied in commercial instruments. Various alkanes and aromatic compounds were subjected to carbon isotope analysis with several types of combustion reactor to illustrate in detail the effects of the reactor on the chromatography of organic compounds. Relatively small quantities of catalyst packed into the reactor, which result in a high linear velocity of carrier gas and an eliminated diffusional broadening of the analytes in the reactor, could improve the peak resolutions of various compounds. However, the improvements could be gained on the peak resolutions, by various types of reactors, are limited. In comparison, the sensitivities for organic compounds might vary greatly with a number of factors, which is mainly attributed to the changes in split ratio at the open split that is closely related with the total flow rate of carrier gas in the reactor.
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    Cited: Baidu(329)
    Synthesis and Characterization of Biodegradable Poly(butylene succinate-co-butylene methyl succinate)
    SUN Yuan-Bi, Xu-Jun, Xu-Yong-Xiang, Yan-Li-Tang, Guo-Bao-Hua
    Chemical Journal of Chinese Universities    2006, 27 (2): 360-364.  
    Abstract2645)      PDF(pc) (429KB)(238)       Save

    Abstract A series of polyesters PBSM, poly(butylene succinate-co-butylene methyl succinate), were obtained by direct melting polycondensation of  succinate and methyl succinic acid with 1,4-butanediol. The compositions and physical properties of the resulted homopolyester and copolyesters were investigated by 1H NMR, differential scanning calorimetry(DSC)and X-ray diffraction. The results suggest that the introduction of comonomer containing a side-chain methyl group led to a change in thermal properties and crystallization behavior. The DSC analysis indicates that with the increase of comonomer content, the Tg, Tm, T0m and crystallinity were decreasing gradually, and the depression of Tm followed Flory′ prediction for random copolymer. Furthermore, an Avrami method was used to analyze the kinetics of isothermal crystallization of PBS and PBSM-20. The Avrami exponents, estimated by Avrami plots, ranging from 2.8 to 3.0 for PBS and 2.7 to 3.0 for PBSM-20 indicate that the mechanism of crystallization for both homopolyester and copolyester was a tridimensional growth with heterogeneous nucleation. Meanwhile, X-ray analysis shows that there was almost no effect of the methyl succinate unit on the crystal structure.

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    Cited: Baidu(178)
    Interactions Between Fluoroquinolones and Bovine Serum Albumin by Fluorescence Method and Affinity Capillary Electrophoresis
    ZHANG Li-Wei, ZHANG Xin-Xiang*
    Chemical Journal of Chinese Universities   
    Abstract2691)      PDF(pc) (519KB)(639)       Save
    The interactions between fluoroquinolones(sparfloxacin, lomefloxacin, norfloxacin, levofloxacin, fleroxacin and pefloxacin) and bovine serum albumin were investigated by affinity capillary electrophoresis and fluorescence quenching method. The binding molar ratio was 1∶1 and the values of binding constants were all at the magnitude level of 104 L/mol. Both van der Waals interaction and hydrogen bonds were involved in the binding process of these fluoroquinolones to BSA. The ACE results also reveal that with the increasing of buffer pH values and ionic strength, the interaction strength became weaker to a certain extent. The FL results and UV-Vis spectrum indicate that the fluorescence quenching was mainly arisen from static quenching by complex formation. The obtained results of these two methods may help us in gaining some insights on possible fluoroquinolones/BSA interactions and in evaluating the drugs’ pharmacokinetic profiles.
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    Cited: Baidu(138)
    Resonance Rayleigh Scattering Spectral Method for Determination of Methylene Blue with Gold Nanoparticle as Probe
    LU Qun-Min, HE You-Qiu, LIU Shao-Pu*, LIU Zhong-Fang
    Chemical Journal of Chinese Universities    2006, 27 (5): 849-852.  
    Abstract2099)      PDF(pc) (201KB)(571)       Save

    In a neutral or weak alkaline medium(pH=6.5-9.5), the gold nanoparticle can combine with methylene blue by the virtue of electrostatic and hydrophobic interaction, forming aggregate with bigger diameters(average diameter increase from 12 to 20 nm ). The aggregate arouse Resonance Rayleigh Scattering(RRS) intensity enhancing greatly. The maximum scattering peaks are at 371 nm. Under optimum conditions, there is a linear relationship between scattering intensity(ΔI) and the concentration of methylene blue. This method has a high sensitivity. So gold nanoparticle can be used as the RRS probe of high sensitivity for methylene blue. The detection limit of methylene blue is 21.17 ng/mL. The method which is simple and rapid has good selectivity. It was successfully applied to the detection of methylene blue in clinic serum samples.

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    Cited: Baidu(104)
    Synthesis and Characterization of Novel Soluble Poly(aryl ether ketone)s
    LIU Bai-Jun, CHEN Chun-Hai, JIN Yu-Hui, HU Wei, SUN Hui, WU Zhong-Wen, JIANG Zhen-Hua, ZHANG Wan-Jin
    Chemical Journal of Chinese Universities    2002, 23 (2): 324-326.  
    Abstract1532)      PDF(pc) (580KB)(179)       Save
    Two novel poly(aryl ether ketone)s based on (3-methyl)phenylhydroquinone were synthesized via aromatic nucleophilic substitution reaction. The high molecular polymers were easily obtained because of the high reaction activity of bisphenol monomer. The traces of DSC showed that the Tgs of m-TPEEK and m-TPEEKK were 421 and 432 K, respectively. The two polymers exhibit a high thermal stability and good solubility. The transparent and flexible films were readily prepared with chloroform solution. The film of m-TPEEK had a low dielectric constant(ε =27).
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    Cited: Baidu(103)
    Synthesis and Properties of Core-shell Fluorosilicone-containing Acrylate Latexes
    HE Ling, XU Yan, ZHU Jiang-Gan, LIANG Jun-Yan*
    Chemical Journal of Chinese Universities   
    Abstract2485)      PDF(pc) (767KB)(635)       Save
    The core-shell silicon-containing fluorinated acrylate latex was obtained via semi-continuous seed emulsion polymerization in which butyl acrylate(BA) served as the core, methyl methylacrylate(MMA), methyl dodecafluorinacrylate(DFHMA in commercial name), 3-methacryloxypropyltrimethoxysilane(MPTMS) and methyltrimethoxysilane(MTMS)(BA/MMA/DFHMA MPTMS/MTMS) served as the shell of copolymer. FTIR, SEM-EDX, and DSC were used not only to analyze the properties of the latexes and films, but also to investigate the effect of DFHMA and MPTMS/MTMS content on the latexes and films. TEM was employed for characterizing the morphology structure and the particle size of the core-shell latex. The results indicate that the copolymers presented uniform spherical core-shell partials with 20—30 nm in diameter, the content of F and Si element on the surface of films have a great effect on the characteristics of the films, and when m(DFHMA)/m(MPTMS+MTMS)=3/1, the film shows much more favorable characteristics both in latex and in film.
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    Cited: Baidu(98)
    Desorption Electrospray Ionization Mass Spectrometry for Direct Analysis of Clinic Urine Samples
    CHEN Huan-Wen1, LI Ming1, ZHOU Jian-Guang1, FEI Qiang1, JIANG Jie1, JIN Qin-Han1, ZHANG Tian-Mu2, ZHANG Xie3
    Chemical Journal of Chinese Universities   
    Abstract2312)      PDF(pc) (335KB)(650)       Save
    DESI-MS was applied to direct simultaneous detection of multiple components of clinic urine samples without any sample pretreatment. Under the optimized working conditions, such as ESI infusion rate, ESI high voltage, incident angle, collective angle, tube lens voltage, etc., for both DESI and LTQ mass spectro-meter, the main components of urine including urea, pyruvic acid, creatinine, oxalic acid, alloxane, menadione were detected as the protonated molecules in positive detection mode using methanol-water(volume ratio 1:1) as the spray solvent in the low mass range(15—200 amu). Sodium and potassium were also detected but mainly in the form of clusters with urea and creatinine. In each case, the corresponding ions were isolated in the ion trap mass analyzer and underwent a collision-induced dissociation process, which yielded characteristic fragments in tandem mass spectra and resulted in confident validation of the analytical results. The average time for single sample analysis was less than 1 min since it required no sample pretreatment. Furthermore, the semi-quantitative analysis of the components was also demonstrated by adding serine as an internal standard into the samples.
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    Cited: Baidu(98)
    Novel Surface-enhanced Resonance Raman Scattering Probe for Nitric Oxide
    LUO Chun-Hua, WU Zhao-Yang*, SHEN Guo-Li, YU Ru-Qin
    Chemical Journal of Chinese Universities   
    Abstract2558)      PDF(pc) (464KB)(689)       Save
    A novel diamino-azobenzene dye was designed and synthesized as a Raman indicator for NO. The Raman chemical transformation of the diamino-azobenzene structure is based on the reactivity of diamines with NO in the presence of dioxygen. The N-nitrosation of the diamino-azobenzene, yielding the benzotriazole-based compounds which exhibit a strong propensity to bind to Ag nanoparticles, offers a simple protocol for the direct detection of NO. As the addition of NO, the SERS spectra of the system changed evidently in the range of 1200—1700 nm and turned out a strong SERS peak at 1300 nm. The effects of the concentration of the dye, the aggregation of the nanoparticles and the pH of the solution were evaluated in detail. The result shows that the detection limit of the SERS probe reaches 10-8 mol/L and the system is independent of pH in the range of 4.5—7.5.
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    Cited: Baidu(86)
    Synthesis and Antifungal Activity of Novel Triazole Derivatives
    SUN Qing-Yan*, CAO Yong-Bing, XU Jian-Ming, ZHANG Wan-Nian, ZHANG Jun, WU Qiu-Ye, ZHANG Da-Zhi, JIANG Yuan-Ying
    Chemical Journal of Chinese Universities   
    Abstract2594)      PDF(pc) (251KB)(832)       Save
    A series of 1-(1H-1,2,4-triazol-1-yl)-2-(2,4-difluorophenyl)-3-[(4-substitutedphenyl)-piperazin-1-yl]-propan-2-ols were designed and synthesized on the basis of the active site of fungal Lanosterol 14α-demethylase(CYP51), the structure-activity relationships and antimycotic mechanism of azole antifungal agents. Their structures were confirmed via elemental analysis, IR, MS and 1H NMR. The results of preliminary antifungal tests against eight human pathogenic fungi(Candida albicans, Candida parapsilosis, Candida tropicalis, Cryptococcus neoformans, Aspergillus fumigatus, Trichophyton rubrum, Fonsecaea compacta, Microsporum gypseum) in vitro show that all compounds exhibited higher activities against fungi than that of fluconazole, voriconazole and amphotericin B; compounds 4a, 4b and 4d showed higher activities against Aspergillus fumigatus than fluconazole and voriconazole(with the MIC values of 0.25, 0.25 and 0.25 μg/mL respectively). For antifungal activity of these novel triazole derivatives, it is very helpful to introduce the 4-(4-substitutedphenyl) piperazine as side chains to interact with the residues of the narrow hydrophobic cleft of CYP51 and adjust the physico-chemical properties of title molecules.
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    Cited: Baidu(84)
    Synthesis of Amphiphilic Chitosan Derivatives and Their Self-aggregation Phenomenon
    WANG Zheng*, TU Chun-Ling
    Chemical Journal of Chinese Universities   
    Abstract2111)      PDF(pc) (664KB)(490)       Save
    A series of chitosan derivatives were synthesized via mPEG as hydrophilic group, sebacic acid as hydrophobic groups. Chitosan derivatives were characterized by FTIR, 1H NMR and XRD. The degree of substitution(DS) was calculated by elemental analysis(EA). Chitosan derivatives were dissolved in double-distilled water to form micelles. The morphology of polymer micelles was measured by transmission electron microscopy(TEM), and the size and distribution of polymer micelles was determined by dynamic light scattering(DLS). The critical aggregation concentration(CAC) was detected by a fluorescence technique using pyrene as a probe. It was found that the CAC was decreased by increasing the DS of acyl group, meanwhile, the size of polymer micelles was decreased.
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    Cited: Baidu(83)
    Analysis of Tobacco by Near-infrared Spectroscopy and Support Vector Machine
    ZHANG Yong, CONG Qian, XIE Yun-Fei, ZHAO Bing*
    Chemical Journal of Chinese Universities    2009, 30 (4): 697-700.  
    Abstract2387)      PDF(pc) (347KB)(270)       Save

    In this study, in order to establish analysis models of near-infrared spectroscopy(NIR) of tobacco, 120 samples of tobacco from different cultivation area were surveyed by near-infrared(NIR) spectroscopy. As the new pattern recognition, support vector machine(SVM) can avoid over-fitting problem and owns the superior generalization ability and prediction accuracy, were applied in this study. The quantitative and qualitative analysis models of tobacco samples were studied separately in this experiment using radial basis function(RBF) SVM. For reducing dimension and moving noise, the spectrum variables were highly effectively compressed using the wavelet transformation(WT) technology and the haar wavelet was selected to decompose the spectroscopy signals. Simultaneously, the parameters of the models were also discussed in detail. The best experimental results were obtained using the RBF SVM regression with kernel parameter σ=1.0, 1.2, 1.4, 0\^6, separately corresponds to total-sugar, reducing sugar, nicotine, total-nitrogen, and RBF SVM classifier with kernel parameter σ=1.6. Meanwhile, the values of appraisal index, namely coefficient of determination(R2), root mean squared error of prediction(RMSEP) and mean relative error(RME), indicate its excellent generalization for quantitative and qualitative analysis results and high prediction accuracy. The overall results show that NIR spectroscopy combined with SVM can be efficiently utilized for rapid and accurate analysis of chemical compositions in tobacco and discrimination of tobacco of different origins. On the other hand, the research can show that SVM is effective modeling tools to NIR spectroscopy and can provide technical support for quantitative and quantitative analysis of other NIR applications.

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    Cited: Baidu(82)
    Synthesis of Eu(Ⅲ) and Tb(Ⅲ) Complexes with Novel Pyridine-2,6-Dicarboxylic Acid Derivatives and Their Fluorescence Properties
    TANG Rui-Ren, YAN Zi-Er, GUO Can-Cheng, LUO Yi-Ming
    Chemical Journal of Chinese Universities    2006, 27 (3): 472-477.  
    Abstract2418)      PDF(pc) (444KB)(404)       Save

    Starting from pyridine-2,6-dicarboxylicacid(DPA),a series of novel pyridine-2,6-dicarboxylic acid derivatives were synthesized. In these compounds,4-(hydroxymethyl)pyridine-2,6-dicarboxylate(4-HMDPA) and 4-{[bis(carboxymethyl)amino] methyl}pyridine-2,6-dicarboxylate(4-BMDPA) were used as multifunctional ligands to coordiate with Tb(Ⅲ) and Eu(Ⅲ) and their complexes were prepared. The fluorescence properties of the solid complexes and their solutions were investigated in detail. The results indicate that the weak election-withdrawing group 4-hydroxymethyl in 4-position of pyridine in 4-HMDPA could weaken the fluorescence intensity of the lanthanide complexes. The contradistinctive experimental results show that the fluorescence intensities of these complexes are related to pH value of the aqueous solution and the dipole moment of solvent molecule: in the neutral aqueous solution,the fluorescence intensities of these complexes were strongest,while the less the dipole moment was,the stronger the fluorescence intensity was. 4-BMDPA is the better sensitizer and may be used as time-resolved fluorommunoassay.

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    Cited: Baidu(82)
    Stereoselective Polymerization of rac-Lactide Initiated by Achiral Schiff-base Isopropoxide Aluminum Complex
    YANG Yong-Kun, Tang-Chao-Hui, PANG-Hui, Du-Hong-Zhi, Chen-Xue-Si, Jing-Xia-Bin
    Chemical Journal of Chinese Universities    2006, 27 (2): 352-355.  
    Abstract2388)      PDF(pc) (350KB)(297)       Save

    Abstract An achiral Schiff-base isopropoxide aluminum complex(Ⅱ) was used for the stereoselective ring-opening polymerization of rac-lactide. The kinetics studies indicated that rac-lactide polymerization was first order kinetics to monomer concentration. There was linear relationship between the monomer conversion and molecular weights(Mn) of the polymer with a narrow molecular distribution. These phenomena indicated that the polymerization was well controllable. Moreover, the obtained poly(rac-lactide) was crystalline polymer with relative high tm(179 ℃). 13C NMR and homonuclear decoupled 1H NMR spectra revealed that the polymerization of rac-lactide initiated by complex(Ⅱ) resulted in the isotactic stereoblock polymer, which contained blocks with an average of 11 units of enantiomerically pure lactic acid.

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    Cited: Baidu(75)
    Electrochemistry and Electrocatalysis of Hemoglobin with SiO2 Gel Film Layer-by-layer Assembled on Carbon Nanotubes-Au Nanoparticles Modified Electrode
    XU Ying, ZHANG Xiao-Yan, YANG Jing*, HE Pin-Gang*, FANG Yu-Zhi
    Chemical Journal of Chinese Universities    2011, 32 (10): 2293-2300.  
    Abstract2925)      PDF(pc) (1337KB)(255)       Save
    Protein direct electrochemistry study and its electro\|catalysis analysis were introduced,  involving layer-by-layer alternate assembly of hemoglobin(Hb)and SiO2 gel film onto electrode surface. The electrode was firstly modified with the nano-compound of multi-walled carbon nanotubes and Au nanoparticles, i.e., MWNTs-Au/GC electrode. Then Hb and SiO2 gel film were alternately spread onto the electrode surface to stabilize the protein and its amount and bioactivity, thus resulting {SiO2/Hb}n/MWNTs-Au/GC electrode. Under the optimized n=2, the Hb on the {SiO2/Hb}2/MWNTs-Au/GC electrode displayed its intrinsic bioactivity well, transferring electrodes with electrode and catalyzing H2O2 reduction as one peroxidaze enzyme.
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    Cited: Baidu(73)
    Kinetics and Thermodynamics of Adsorption of Phenolonto Mesoporous Carbon CMK-3
    GUO Zhuo1, YUAN Yue2
    Chemical Journal of Chinese Universities   
    Fluorescence Spectrum Study of Sol-gel Transition in Alginate Aqueous Solutions Induced by Calcium Cations
    LU Lu1, LIU Xin-Xing2, TONG Zhen2*
    Chemical Journal of Chinese Universities   
    Abstract2366)      PDF(pc) (276KB)(561)       Save
    In order to establish an experiment method to determine the gelation point for the physical gelation without disturbing the system mechanically, the fluorescence spectrum was used to monitor the sol-gel transition in the aqueous solutions of FITC labeled alginate induced by Ca2+. The slope change was found from the curves of the emission strength and fluorescence anisotropy against gelation time, indicating the gelation time of 80 min, which just equaled that determined by rheology measurement. The label fluorescence strength and anisotropy can be used to determine the gel point for the physical gelation.
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    Cited: Baidu(68)
    Surface Desorption Atmospheric Pressure Chemical Ionization Mass Spectrometry for Direct Detection of Trace Amounts of Cocaine in Hot Pot Sauce Materials
    SONG Qing-Hao, WANG Jiang, HU Bin, CHEN Huan-Wen, JIN Qin-Han*
    Chemical Journal of Chinese Universities    2010, 31 (10): 1961-1964.  
    Abstract2374)      PDF(pc) (470KB)(292)       Save
    A novel method was developed for the direct detection of cocaine in hot pot sauce materials by surface desorption atmospheric pressure chemical ionization mass spectrometry(SDAPCI-MS) without any sample pretreatment. By using sample needle sampling, the volume of each sampling was at nanoliter level. The ave-rage time for a single sample analysis was less than 0.5 min. The recoveries of six samples spiked with cocaine were shown to be in the range of 92.9%—106.6%, and the relative standard deviations of the method were in the range of 5.2%—11.8%. The detection limit of this method for cocaine was found to be 1.5×10-12 g/mL. The data show SDAPCI-MSn is a powerful tool for rapid, semi-quantitative detection of cocaine in hot pot sauce materials.
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    Cited: Baidu(66)
    Simultaneous Adsorption of Organic Pollutant and Heavy Metal onto Surfactant-Modified Organobentonites with Chelating Ligands
    SUN Hong-Liang1,2*, ZHU Li-Zhong1
    Chemical Journal of Chinese Universities   
    Abstract2448)      PDF(pc) (437KB)(836)       Save
    The surfactant-modified organobentonites with chelating ligands, IMB-CTMA-Am, were synthesized, where IMB refers to natural bentonite obtained from Inner Mongolia of China, CTMAB refers to quaternary ammonium cation surfactant of cetyltrimethylammonium bromide, and Am refers to the chelating ligands, respectively. The adsorbent samples were characterized by X-ray diffraction(XRD), thermogravimetric and differential thermal(TG-DTA) analyses, specific surface area(N2-BET) measurements, and elemental analysis. The results indicated that CTMA+ and Am intercalated into the lamellae of bentonites successfully. The adsorption experiments showed that IMB-CTMA-Am could effectively adsorb organic pollutant p-nitrophenol(PNP) and heavy metal ion Pb2+ in waste water system simultaneously. The adsorption capabilities of IMB-CTMA-Am are greater than natural bentonite IMB and modified bentonite IMB-CTMA. Fourier transform infrared(FTIR) spectrum study revealed that the N—H vibrational frequency of IMB-CTMA-Am was downshifted after Pb2+ adsorption, which demonstrates the formation of a metal complex between metal ion Pb2+ and Am in the interlayers of the modified bentonites. The adsorption capacity of Pb2+ onto IMB-CTMA-Am agrees with the stability constant of the complex formed.
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    Cited: Baidu(65)
    Synthesis and Characterization of Novel Sulfonated Poly(arylene ether nitrile ketone)s Containing Dicyanoarylene Group
    CHEN Yong, WANG Shuan-Jin, XIAO Min, MENG Yue-Zhong
    Chemical Journal of Chinese Universities   
    Abstract2532)      PDF(pc) (366KB)(573)       Save
    A novel monomer of bisphenol containing dicyanoarylene group was synthesized and followed by copolymerization with activated dihalides to give a series of sulfonated poly(arylene ether nitrile ketone)s with a high molecular weight. The structures of the copolymers were characterized by 1H NMR and elemental analysis. The acid-form membranes of the copolymers exhibited an excellent thermostability, good proton conducti-vity, dimensional and chemical stabilities as well as superior mechanical strength demonstrated by the corresponding technologies available. Which denomstrate the membranes prepared are promising candidate for PEMFC application.
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    Cited: Baidu(64)
    Supramolecular Structure, Thermal Stability and Release Property of New Drug-inorganic Composites Norfloxacin-intercalated Mg-Al-layered Double Hydroxides
    NI Zhe-Ming*, XIA Sheng-Jie, WANG Li-Geng, XING Fang-Fang, PAN Guo-Xiang, HU Jun
    Chemical Journal of Chinese Universities   
    Abstract2450)      PDF(pc) (662KB)(927)       Save
    A new drug-inorganic composite involving an antibiotic compound norfloxacin(Nor) intercalated Mg-Al layered double hydroxides(Nor-LDHs) was assembled with coprecipitation and ion-exchange methods. The samples thereby obtained were characterized via XRD, FTIR, UV-Vis, TG-DTA and ICP measurements. The results show that the original interlayer nitrate anions of the hydrotalcite can be replaced by norfloxacin anions, and norfloxacin intercalated Mg-Al layered double hydroxides were obtained with a good crystallinity. XRD analyses indicates that the interlayer spaces of as-synthesized Nor-LDHs were 1.29 nm to 1.33 nm, and compared with three-dimensional molecular size of Nor ion calculated from the PM3 semi-empirical molecular orbital method. The norfloxacin guests were arranged alternately with monolayer vertical(along the short axis orientation) between layers. It is found that the interaction of the host layers and the guests is through hydrogen bonding and electrostatic attraction, confirming that the intercalated hydrotalcite has a supramolecular structure. The thermal stability, acid resistance and sustained-release of norfloxacin anion-pillared hydrotalcite were enhanced to a considerable extent, comparing with that of norfloxacin. The release profiles were fitted by Bhaskar equation and the first-order equation, the fitting data primarily follow the experimental results.
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    Cited: Baidu(61)