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1.
Microcrystalline cellulose (MCC) particles were subjected to hydrothermal treatment using an autoclave with temperatures ranging from 200 to 250 °C and reaction times ranging from 20 to 100 min. The structure and chemical composition of the reacted solid phase was analyzed by X-ray diffraction, thermo-gravimetric analysis, FTIR spectroscopy and 13C-NMR spectroscopy. The relative composition of the water-soluble products was determined by one-dimensional 1H-NMR and two-dimensional homo and hetero-nuclear NMR spectroscopy. Within the experimental temperature and treatment time ranges, the crystallinity of the reacted solid phase was found to be mostly dependent on the treatment temperature while the aqueous solution was found to change with both temperature and treatment time. At the maximum temperature employed in this study (250 °C), the solid products are similar to amorphous oxidized carbon with glucose as the main water-soluble product. At lower temperatures the particles are unconverted MCC and the liquid products are primarily levulinic acid, formic acid and acetic acid with smaller quantities of 5-hydroxymethyl-furfural and glucose. Heterogeneous and liquid phase reaction-schemes are proposed to explain the observed solid and water-soluble products as a function of temperature and treatment time.  相似文献   

2.
A pilot study was carried out to evaluate the scope of instrumental neutron activation analysis (INAA) for measuring the levels of selected elements in a few commonly consumed food items in Thailand. Several varieties of rice, beans, aquatic food items, vegetables and soybean products were bought from major distribution centers in Bangkok, Thailand. Samples were prepared according to the protocols prescribed by the nutritionist for food compositional analysis. Levels of As, Br, Ca, Cd, Cl, Cr, Cu, Fe, K, Mg, Mn, and Zn were measured by INAA using the irradiation and counting facilities available at the Thai Research Reactor with the maximum in-core thermal neutron flux of 3 × 1013 cm?2 s?1 of the Thailand Institute of Nuclear Technology in Bangkok. Selenium was determined by cyclic INAA using the Dalhousie University SLOWPOKE-2 Reactor facilities in Halifax, Canada at a thermal neutron flux of 2.5 × 1011 cm?2 s?1. Both cooked and uncooked foods were analyzed. The elemental composition of food products was found to depend significantly on the raw material as well as the preparation technique.  相似文献   

3.
Thermal decomposition of magnesite is investigated by using a TG–MS. Different kinetic methods including Coats–Redfern, Flynn–Wall–Ozawa, and Kissinger–Akahira–Sunose are used to investigate the thermal decomposition kinetics of magnesite. It was observed that the activation energy values obtained by these methods are similar. The average apparent activation energy is found to be about 203 kJ mol?1. The raw magnesite and its decomposition products obtained at different temperatures are analyzed by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscope (SEM). The concentration of functional groups, crystal structure and composition, and apparent morphology of decomposition products were studied in detail. The FTIR, XRD, and SEM analyses showed that magnesite was completely decomposed at 973 K to form MgO.  相似文献   

4.
A stability-indicating ultra-high-performance liquid chromatography (UHPLC) method with a diode array detector was developed and validated for the determination of cis/trans isomers of perindopril l-arginine in bulk substance and pharmaceutical dosage form. The separation was achieved on a Poroshell 120 Hilic (4.6 × 150 mm, 2.7 µm) column using a mobile phase composed of acetonitrile–0.1 % formic acid (20:80 v/v) at a flow rate of 1 mL min?1. The injection volume was 5.0 µL and the wavelength of detection was controlled at 230 nm. The selectivity of the UHPLC-DAD method was confirmed by determining perindopril l-arginine in the presence of degradation products formed during acid–base hydrolysis and oxidation as well as degradation in the solid state, at an increased relative air humidity and in dry air. The method’s linearity was investigated in the ranges 0.40–1.40 µg mL?1 for isomer I and 0.40–2.40 µg mL?1 for isomer II of perindopril l-arginine. The UHPLC-DAD method met the precision and accuracy criteria for the determination of the isomers of perindopril l-arginine. The limits of detection and quantitation were 0.1503 and 0.4555 µg mL?1 for isomer I and 0.0356 and 0.1078 µg mL?1 for isomer II, respectively.  相似文献   

5.
A major enhancement of grease and water vapor barrier properties was accomplished with a 1–10 g/m2 coating of O-acetyl galactoglucomannan (GGM) ester or with GGM coatings applied as water dispersions on cartonboard. GGMs were esterified with phthalic and benzoic anhydrides, respectively. The novel phthalic esters of GGM (GGM-Ph) were characterized with HPLC, NMR, and matrix-assisted laser desorption/ionization with mass spectrometry (MALDI-TOF-MS). The degree of substitution of GGM-Ph was obtained by 1H NMR, 13C NMR, and HPLC. The GGM esters and GGM were coated onto cartonboard, and they demonstrated good moisture and very good grease resistance even with thin 1–3 g/m2 coatings. The time for penetration of 0.1 % rapeseed oil was 54 h with the 2.4 g/m2 coating thickness. The lowest water vapor transmission value was 39 g/m2/24 h with 9.7 g/m2 coating. The GGM esters had clearly higher water resistance and slightly higher grease barrier values than native GGM. High-molar-mass-based GGM (50 kg/mol) and GGM-Ph rendered better water vapor and grease barrier properties than low-molar-mass GGM (9 kg/mol) and GGM-Ph. The GGM-based coatings can be safely used on an industrial scale as water was used as a solvent. As obtained from non-food-based side-stream wood-based resources, GGM and GGM esters project a sustainable and modern conception for barrier purposes in food packaging.  相似文献   

6.
Ultraperformance convergence chromatography/tandem triple quadrupole mass spectrometry (UPC2-MS/MS) is a novel tool in separation science that combines the advantages of supercritical fluid chromatography with ultraperformance liquid chromatography/MS/MS technology. The use of nontoxic CO2 fluid and a postcolumn additive to complement MS/MS allows better control of analyte retention for chiral separation and high-sensitivity determination with different chiral stationary phases. This paper reports the stereoselective separation and determination of the chiral neonicotinoid sulfoxaflor in vegetables and soil by UPC2-MS/MS. Baseline resolution (Rs?≥?1.56) of and high selectivity (LOQ?≤?1.83 μg/kg) for the four stereoisomers were achieved by postcolumn addition of 1 % formic acid–methanol to a Chiralpak IA-3 using CO2/isopropanol/acetonitrile as the mobile phase at 40 °C, 2,500 psi, and for 6.5 min in electrospray ionization positive mode. Rearranged Van’t Hoff equations afforded the thermodynamic parameters ΔH ο and ΔS ο, which were analyzed to promote understanding of the enthalpy-driven separation of sulfoxaflor stereoisomers. The interday mean recovery, intraday repeatability, and interday reproducibility varied from 72.9 to 103.7 %, from 1.8 to 9.2 %, and from 3.1 to 9.4 %, respectively. The proposed method was used to study the pharmacokinetic dissipation of sulfoxaflor stereoisomers in soil under greenhouse conditions. The estimated half-life ranged from 5.59 to 6.03 d, and statistically nonsignificant enantioselective degradation was observed. This study not only demonstrates that the UPC2-MS/MS system is an efficient and sensitive method for sulfoxaflor stereoseparation, but also provides the first experimental evidence of the pharmacokinetic dissipation of sulfoxaflor stereoisomers in the environment. Graphical Abstract
Chemical structure and UPC2-MS/MS separation chromatogram of sulfoxaflor. (* stereogenic center)  相似文献   

7.
Thermal behaviour of heptakis-6-iodo-6-deoxy-beta-cyclodextrin (HIDBCD) under inert and oxidative conditions was investigated by TG/DTG/DTA, FTIR, and using the hyphenate technique TG–FTIR. Due to the fact that thermal behaviour of HIDBCD was not studied before, we set our goal in the investigation of thermal degradation process in a dynamic air atmosphere vs. nitrogen atmosphere at a heating rate of 10 °C min?1, up to 500 °C, respectively, 600 °C. It was found that the degradation process in air occurs in a single step, with a total mass loss of 99.9 %. The results of TG/DTG/DTA–FTIR indicated that the thermal behaviour of this cyclodextrin can be divided into three stages and more information was provided about the reaction sequences and the relevant products of reaction.  相似文献   

8.
In order to improve the antimicrobial activity of bacterial cellulose (BC), the silver nanoparticles (Ag NPs) were in situ fabricated on the BC membranes, affording BC and Ag hybrid antimicrobial materials, BC + Ag, which possesses excellent antimicrobial performance. Typically, carboxyl groups were firstly introduced into BC by TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl radical)-mediated oxidation. Then, the carboxyl-functionalized BC was performed with ion-exchange reaction to change the sodium ions into Ag+ by immersing in AgNO3 aqueous solution, generating Ag+ anchored BC. Finally, two types of distinct reductive reagents including NaBH4 and sodium citrate were employed to transform Ag+ into Ag NPs to fabricate BC + Ag. The diameters of Ag NPs were determined to be 3.8 nm for NaBH4-reduced BC + Ag, and 22.0 nm for sodium citrate-reduced one, respectively. The silver content of BC + Ag were determined to be 1.944 and 2.895 wt% for NaBH4-reduced sample and sodium citrate-reduced one, respectively. Two types of BC + Ag both showed a slow and persistent Ag+ release profile, but the NaBH4-reduced one released much more Ag+ than that of sodium citrate under the same measurement condition. In-depth antibacterial analysis via the disc diffusion and colony forming count method disclosed that BC + Ag exhibited strong bactericidal effects against both Escherichia coli and Staphylococcus aureus. And the antibacterial activity of NaBH4-reduced BC + Ag was higher than the sodium citrate-reduced one. Overall, this study would further improve the antibacterial efficiency of BC + Ag.  相似文献   

9.
A selective, rapid, accurate and precise stability-indicating RP-HPLC method was developed for monitoring vilazodone in the presence of its degradation products (DPs) in API and pharmaceutical dosages. Chromatographic separation was achieved using a Grace phenyl C18 column (250 × 4.6 mm, 5 µm particle size) at a flow rate of 1.0 mL min?1 with a linear gradient elution of ammonium acetate buffer (10 mM, pH 5.0 adjusted by acetic acid) with acetonitrile as the mobile phase. Detection was performed at 240 nm. The chromatographic conditions were optimized by the design of experiments to obtain the best possible separation with a minimum number of trials. A face-centered central composite design (three levels for each factor) was employed for optimization, and an interaction of the independent variables (pH of mobile phase, column temperature and  % of organic modifier) on the resolution of critical pairs was studied. The drug was subjected to the stress conditions of hydrolytic (acid, base and neutral), oxidative, thermal and photolytic degradation. It was found to be degraded significantly in hydrolytic (basic and acid) and oxidative conditions, while it was stable in neutral hydrolytic, thermal and photolytic conditions. LC-QTOF/MS/MS studies were carried out to characterize the major DPs. The method was fully validated for selectivity, linearity, accuracy, precision and robustness in compliance with ICH guideline Q2 (R1).  相似文献   

10.
A certified reference material (CRM) for the determination of perfluorooctanoic acid (PFOA) has been issued as NMIJ CRM 4056-a by the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Purity (kg kg?1) based on a titration method was determined by subtracting the mass fractions of impurities measured using liquid chromatography/mass spectrometry (LC/MS) from those of acids expressed as PFOA measured by a neutralization potentiometric titration. To validate an obtained result, purity based on a mass balance method was determined by subtracting the mass fractions of impurities, measured using LC/MS, Karl-Fischer titration (KFT), and vacuum evaporation, from 1 kg kg?1. Results from both titration and mass balance methods were in agreement within the accepted limits of uncertainty. The certified purity of NMIJ CRM 4056-a was determined to be 0.959 kg kg?1, calculated as the mean of the results obtained with the two methods. The standard uncertainty of the certified purity was evaluated from purity evaluations as well as from sample homogeneity and stability obtained from LC/MS and KFT analyses. Consequently, the expanded uncertainty was estimated to be 0.005 kg kg?1 with a coverage factor of k = 2.  相似文献   

11.
ZnS nanoparticles implanted with 45 keV O5+ ion beam exhibited 83.6 % degradation of methyl blue in 2 h. This idea was utilized to fabricate nanocomposite system of ZnS and PMMA where ZnS nanoparticles were immobilized in PMMA film and irradiated with 45 keV O5+ ion beam at particle fluence of 2.5 × 1015, 1 × 1016 and 4 × 1016 particles/cm2. These irradiated batches of ZnS nanoparticle immobilized in PMMA batches revealed formation of porous structure characterized by scanning electron microscopy and these batches exhibited 54 % photocatalytic degradation of methyl blue in 80 min which was higher as compared to the pristine ZnS nanoparticles.  相似文献   

12.
Xanthine oxidase (XOD) catalyzes the metabolism of hypoxanthine and xanthine to uric acid, the overproduction of which could cause hyperuricemia, a risk factor for gout. Inhibition of XOD is a major treatment for gout, and biflavonoids have been found to act as XOD-inhibitory compounds. In this study, ultrafiltration liquid chromatography with photodiode-array detection coupled to electrospray-ionization tandem mass spectrometry (UF-LC-PDA–ESI-MS) was used to screen and identify XOD inhibitors from S. tamariscina. High-performance counter-current chromatography (HPCCC) was used to separate and isolate the active constituents of these XOD inhibitors. Furthermore, ultrahigh-performance liquid chromatography (UPLC) and triple-quadrupole mass spectrometry (TQ-MS) was used to determine the XOD-inhibitory activity of the obtained XOD inhibitors, and enzyme kinetics was performed with Lineweaver–Burk (LB) plots using xanthine as the substrate. As a result, two compounds in S. tamariscina were screened as XOD inhibitors: 65.31 mg amentoflavone and 0.76 mg robustaflavone were isolated from approximately 2.5 g?S. tamariscina by use of HPCCC. The purities of the two compounds obtained were over 98 % and 95 %, respectively, as determined by high-performance liquid chromatography (HPLC). Lineweaver–Burk plot analysis indicated that amentoflavone and robustaflavone were non-competitive inhibitors of XOD, and the IC 50 values of amentoflavone and robustaflavone for XOD inhibition were 16.26 μg mL?1 (30.22 μmol L?1) and 11.98 μg mL?1 (22.27 μmol L?1), respectively. The IC 50 value of allopurinol, used as the standard, was 7.49 μg mL?1 (46.23 μmol L?1). The results reveal that the method for systematic screening, identification, and isolation of bioactive components in S. tamariscina and for detecting their inhibitory activity using ultrafiltration LC–ESI-MS, HPCCC, and UPLC–TQ-MS is feasible and efficient, and could be expected to extend to screening and separation of other enzyme inhibitors. Graphical Abstract
?  相似文献   

13.
A new metal matrix composite material has been developed to serve as a thermal neutron absorber for testing fast reactor fuels and materials in an existing pressurized water reactor. The performance of this material was evaluated by placing neutron fluence monitors within shrouded and unshrouded holders and irradiating for up to four cycles. The monitor wires were analyzed by gamma and X-ray spectrometry to determine the activities of the activation products. Adjusted neutron fluences were calculated and grouped into three bins—thermal, epithermal, and fast—to evaluate the spectral shift created by the new material. A comparison of shrouded and unshrouded fluence monitors shows a thermal fluence decrease of ~11 % for the shielded monitors. Radioisotope activity and mass for each of the major activation products is given to provide insight into the evolution of thermal absorption cross-section during irradiation. The thermal neutron absorption capability of the composite material appears to diminish at total neutron fluence levels of ~8 × 1025 n/m2. Calculated values for dpa in excess of 2.0 were obtained for two common structural materials (iron and nickel) of interest for future fast flux experiments.  相似文献   

14.
A new method for the growth-dependent headspace analysis of bacterial cultures by needle trap (NT)-gas chromatography-mass spectrometry (GC-MS) was established. NTs were used for the first time as enrichment technique for volatile organic compounds (VOCs) in the headspace of laboratory cultures. Reference strains of Escherichia coli and Pseudomonas aeruginosa were grown in different liquid culture media for 48 h at 36 °C. In the course of growth, bacterial culture headspace was analysed by NT-GC-MS. In parallel, the abiotic release of volatile organic compounds (VOC) from nutrient media was investigated by the same method. By examination of microbial headspace samples in comparison with those of uninoculated media, it could be clearly differentiated between products and compounds which serve as substrates. Specific microbial metabolites were detected and quantified during the stationary growth phase. P. aeruginosa produced dimethyl sulfide (max. 125 μg L?1??1) and 2-nonanone (max. 200 μg L?1), whereas E. coli produced carbon disulfide, butanal and indole (max. 149 mg L?1). Both organisms produced isoprene. Graphical Abstract
MVOCs produced by P. aeruginosa and E. coli at T = 36 °C in autoclaved LB + TRP medium   相似文献   

15.
A series of silica-supported nickel catalyst precursors was synthesized with different SiO2/Ni mole ratios (0.20, 0.80 and 1.15). Non-isothermal reduction of Ni catalyst precursors was investigated by temperature-programmed reduction at four different heating rates (2, 5, 10 and 20 °C min?1), in a hydrogen atmosphere. Kinetic parameters (E a, A) were determined using Friedman isoconversional method. It was found that for all mole ratios, apparent activation energy is practically constant in conversion range of α = 30–70 %. In considered conversion range, the following values of apparent activation energy were found: E a = 129.5 kJ mol?1 (SiO2/Ni = 0.20), E a = 133.8 kJ mol?1 (SiO2/Ni = 0.80) and E a = 125.0 kJ mol?1 (SiO2/Ni = 1.15). Using two special functions (y(α) and z(α)), the kinetic model was determined. It was established that reduction of Ni catalyst precursors with different SiO2/Ni mole ratios is a complex process and can be described by two-parameter ?esták–Berggren (SB) autocatalytic model. Based on established values of SB parameters for each mole ratio, the possible mechanism was discussed. It was found that for all investigated ratios, the Weibull distribution function fits very well the experimental data, in the wide range of conversions (α = 5–95 %). Based on obtained values of Weibull shape parameter (θ), it was found that experimentally evaluated density distribution functions of the apparent activation energies can be approximated by the unbalanced peaked normal distribution.  相似文献   

16.
This work describes a novel polyaniline-magnetite nanocomposite and its application to the preconcentration of Cr(VI) anions. The material was obtained by oxidative polymerization of aniline in the presence of magnetite nanoparticles. The parameters affecting preconcentration were optimized by a Box-Behnken design through response surface methodology. Extraction time, amount of magnetic sorbent and pH value were selected as the main factors affecting sorption. The sorption capacity of the sorbent for Cr(VI) is 54 mg g?1. The type, volume and concentration of the eluents, and the elution time were selected as main factors in the optimization study of the elution step. Following sorption and elution, the Cr(VI) ions were reacted with diphenylcarbazide, and the resulting dye was quantified by HPLC with optical detection at 546 nm. The limit of detection is 0.1 μg L?1, and all the relative standard deviations are <6.3 %. The nanocomposite was successfully applied to the rapid extraction and determination of trace quantities of Cr(VI) ions in spiked water samples. Figure
A schematic procedure of magnetic solid phase extraction  相似文献   

17.
An electrochemical sensor was developed and tested for detection of L-tyrosine in the presence of epinephrine by surface modification of a glassy carbon electrode (GCE) with Nafion and cerium dioxide nanoparticles. Fabrication parameters of a surfactant-assisted precipitation method were optimized to produce 2–3 nm CeO2 nanoparticles with very high surface-to-volume ratio. The resulting nanocrystals were characterized structurally and morphologically by X-ray diffractometery (XRD), scanning and high resolution transmission electron microscopy (SEM and HR-TEM). The nanopowder is sonochemically dispersed in a Nafion solution which is then used to modify the surface of a GCE electrode. The electrochemical activity of L-tyrosine and epinephrine was investigated using both a Nafion-CeO2 coated and a bare GCE. The modified electrode exhibits a significant electrochemical oxidation effect of L-tyrosine in a 0.2 M Britton-Robinson (B-R) buffer solution of pH 2. The electro-oxidation peak current increases linearly with the L-tyrosine concentration in the molar concentration range of 2 to 160 μM. By employing differential pulse voltammetry (DPV) for simultaneous measurements, we detected two reproducible peaks for L-tyrosine and epinephrine in the same solution with a peak separation of about 443 mV. The detection limit of the sensor (signal to noise ratio of 3) for L-tyrosine is ~90 nM and the sensitivity is 0.20 μA μM?1, while for epinephrine these values are ~60 nM and 0.19 μA μM?1. The sensor exhibited excellent selectivity, sensitivity, reproducibility and stability as well as a very good recovery time in real human blood serum samples.
Simultaneous electrochemical determination of L-tyrosine and epinephrine in blood plasma with Nafion-CeO2/GCE modified electrode showing a 443 mV peak-to-peak potential difference between species oxidation peak currents.  相似文献   

18.
Scheelite type BaMoO4 nanofibers were prepared by using acrylamide assisted sol–gel process and electrospinning technique. The prepared Scheelite BaMoO4 nanofibers were characterized by using TG/DTA, XRD, FTIR, FT-Raman and SEM–EDX techniques. Thermal behavior, crystalline phase and structure of the prepared BaMoO4 nanofibers samples were confirmed from the analysis of the obtained results of TG/DTA, XRD, FTIR and FT-Raman respectively. SEM micrographs along with EDX showed the formation of one dimensional (1D) nanofibers 100–350 nm diameters and existence of Ba, Mo and O elements in the BaMoO4 nanofibers sample. The electrical conductivity of BaMoO4 nanofibers as a function of temperature 200–400 °C under air was evaluated by analyzing the measured impedance data using the winfit software. The newly prepared Scheelite type BaMoO4 nanofibers showed electrical conductivity of 0.92 × 10?3 S/cm at 400 °C.  相似文献   

19.
Aminophylline (AMF) was studied as corrosion inhibitor for carbon steel in 1.0 mol L?1 HCl solution using electrochemical measurements associated with UV–Vis spectrophotometry and optical microscopy. Simultaneous thermogravimetry/derivative thermogravimetry and differential scanning calorimetry analysis was performed in order to determine the temperature range in which AMF is an effective inhibitor, without the decomposition risk that could change the inhibition mechanism. Thermal behaviour restricts AMF application as corrosion inhibitor for carbon steel in 1.0 mol L?1 HCl solution at temperatures ≤45 °C where there are no significant modifications of the adsorption mechanism. According to the results of electrochemical measurements, in association with UV–Vis spectrophotometry and optical microscopy techniques, AMF is a mixed-type inhibitor for carbon steel corrosion in 1.0 mol L?1 HCl solution, simultaneously suppressing the anodic and cathodic processes and acting via spontaneous physisorption on the metal surfaces.  相似文献   

20.
BaTiO3:(5 %)Eu3+ nanoparticles and BaTiO3:(5 %)Eu3+@SiO2 composites were synthesized by the solvothermal method. The effects on the structure, morphology and luminescent properties were studied using samples with different molar ratios of BaTiO3:(5 %)Eu3+@SiO2: 60:40, 50:50, 40:60, 30:70, 20:80, 10:90, 08:92, 6.5:93.5, 05:95, and 1.5:98.5. When the amount of silica in the composites was increased, the orange emission of Eu3+ increased, too; this was observed by exciting the charge transfer band centered at 283 nm. Furthermore, an increase in the intensity of the emission was obtained under excitation at 394 nm as a consequence of the improvement in the crystallinity of the samples. The presence of silica and the degree of crystallinity of the samples were determined through the Fourier transform infrared spectra and X-ray diffraction patterns. All of the results suggest that our ceramic material could be a good candidate for biomedical applications such as biolabeling, since the luminescence of BaTiO3:(5 %)Eu3+@SiO2 composites have an emission intensity higher than that of nanoparticles composed solely of BaTiO3:Eu3+. This work demonstrates that BaTiO3:Eu3+@SiO2 composites have an emission intensity higher than that of nanoparticles composed solely of BaTiO3:Eu3+.  相似文献   

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